# Electronic Supplementary Material (ESI) for CrystEngComm. # This journal is © The Royal Society of Chemistry 2017 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_complex2 _database_code_depnum_ccdc_archive 'CCDC 1413539' _audit_update_record ; 2015-07-17 deposited with the CCDC. 2017-07-31 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H48 Ag2 F6 N4 O16 S2' _chemical_formula_sum 'C60 H48 Ag2 F6 N4 O16 S2' _chemical_formula_weight 1474.88 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' Ag Ag -0.8971 1.1015 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2252(16) _cell_length_b 14.362(3) _cell_length_c 24.711(5) _cell_angle_alpha 96.20(3) _cell_angle_beta 96.65(3) _cell_angle_gamma 104.58(3) _cell_volume 2777.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 60421 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 24.10 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.764 _exptl_crystal_F_000 1488 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 0.879 _shelx_estimated_absorpt_T_min 0.830 _shelx_estimated_absorpt_T_max 0.902 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44456 _diffrn_reflns_av_unetI/netI 0.0346 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.480 _diffrn_reflns_theta_max 23.584 _diffrn_reflns_theta_full 23.584 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 8275 _reflns_number_gt 7530 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'X-Area (Stoe & Cie, 2009)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2009)' _computing_data_reduction 'X-RED32(Stoe & Cie, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+52.2093P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8275 _refine_ls_number_parameters 780 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.2101 _refine_ls_wR_factor_gt 0.2081 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9686(10) 0.7372(6) 0.2928(3) 0.0230(18) Uani 1 1 d . . . . . H1 H 1.0160 0.7187 0.3255 0.028 Uiso 1 1 calc R U . . . C2 C 0.7825(11) 0.6993(6) 0.2122(3) 0.0288(19) Uani 1 1 d . . . . . H2 H 0.6963 0.6534 0.1869 0.035 Uiso 1 1 calc R U . . . C3 C 0.8360(11) 0.7926(6) 0.2004(3) 0.0282(19) Uani 1 1 d . . . . . H3 H 0.7868 0.8099 0.1675 0.034 Uiso 1 1 calc R U . . . C4 C 0.9615(11) 0.8609(6) 0.2363(3) 0.0272(19) Uani 1 1 d . . . . . H4 H 1.0001 0.9256 0.2288 0.033 Uiso 1 1 calc R U . . . C5 C 1.0290(10) 0.8325(5) 0.2833(3) 0.0202(17) Uani 1 1 d . . . . . C6 C 1.1647(11) 0.9052(6) 0.3230(3) 0.0249(18) Uani 1 1 d . . . . . C7 C 1.3602(10) 0.9285(6) 0.4061(3) 0.0257(18) Uani 1 1 d . . . . . H7A H 1.4313 0.9777 0.3874 0.031 Uiso 1 1 calc R U . . . H7B H 1.4319 0.8881 0.4205 0.031 Uiso 1 1 calc R U . . . C8 C 1.3023(10) 0.9802(6) 0.4541(3) 0.0202(17) Uani 1 1 d . . . . . C9 C 1.3425(10) 1.0823(6) 0.4645(3) 0.0249(18) Uani 1 1 d . . . . . C10 C 1.4237(11) 1.1438(6) 0.4280(4) 0.0281(19) Uani 1 1 d . . . . . H10 H 1.4494 1.1148 0.3948 0.034 Uiso 1 1 calc R U . . . C11 C 1.4649(12) 1.2420(7) 0.4396(4) 0.036(2) Uani 1 1 d . . . . . H11 H 1.5162 1.2808 0.4141 0.043 Uiso 1 1 calc R U . . . C12 C 1.4315(12) 1.2872(7) 0.4897(4) 0.038(2) Uani 1 1 d . . . . . H12 H 1.4641 1.3561 0.4983 0.045 Uiso 1 1 calc R U . . . C13 C 1.3533(11) 1.2322(6) 0.5252(4) 0.031(2) Uani 1 1 d . . . . . H13 H 1.3307 1.2634 0.5583 0.037 Uiso 1 1 calc R U . . . C14 C 1.3034(10) 1.1279(6) 0.5142(3) 0.0238(18) Uani 1 1 d . . . . . C15 C 1.2190(10) 1.0721(6) 0.5505(3) 0.0221(17) Uani 1 1 d . . . . . C16 C 1.1722(10) 0.9692(6) 0.5394(3) 0.0240(18) Uani 1 1 d . . . . . C17 C 1.0832(11) 0.9071(6) 0.5738(3) 0.0275(19) Uani 1 1 d . . . . . H17 H 1.0528 0.9352 0.6064 0.033 Uiso 1 1 calc R U . . . C18 C 1.0411(11) 0.8088(6) 0.5612(4) 0.030(2) Uani 1 1 d . . . . . H18 H 0.9801 0.7697 0.5847 0.036 Uiso 1 1 calc R U . . . C19 C 1.0856(12) 0.7647(7) 0.5144(4) 0.032(2) Uani 1 1 d . . . . . H19 H 1.0547 0.6958 0.5061 0.038 Uiso 1 1 calc R U . . . C20 C 1.1739(11) 0.8200(6) 0.4802(4) 0.0280(19) Uani 1 1 d . . . . . H20 H 1.2065 0.7888 0.4489 0.034 Uiso 1 1 calc R U . . . C21 C 1.2180(10) 0.9232(6) 0.4904(3) 0.0219(17) Uani 1 1 d . . . . . C22 C 1.1696(10) 1.1226(6) 0.6005(3) 0.0263(19) Uani 1 1 d . . . . . H22A H 1.1082 1.1698 0.5887 0.032 Uiso 1 1 calc R U . . . H22B H 1.0910 1.0738 0.6173 0.032 Uiso 1 1 calc R U . . . C23 C 1.3632(10) 1.1225(6) 0.6810(3) 0.0238(18) Uani 1 1 d . . . . . C24 C 1.4994(10) 1.1878(6) 0.7245(3) 0.0223(17) Uani 1 1 d . . . . . C25 C 1.5584(11) 1.1465(6) 0.7684(3) 0.0271(19) Uani 1 1 d . . . . . H25 H 1.5143 1.0794 0.7703 0.033 Uiso 1 1 calc R U . . . C26 C 1.6826(11) 1.2050(6) 0.8093(3) 0.0288(19) Uani 1 1 d . . . . . H26 H 1.7269 1.1784 0.8394 0.035 Uiso 1 1 calc R U . . . C27 C 1.7407(11) 1.3019(6) 0.8055(3) 0.030(2) Uani 1 1 d . . . . . H27 H 1.8251 1.3418 0.8339 0.036 Uiso 1 1 calc R U . . . C28 C 1.5660(11) 1.2855(6) 0.7231(3) 0.0263(19) Uani 1 1 d . . . . . H28 H 1.5269 1.3127 0.6924 0.032 Uiso 1 1 calc R U . . . C29 C 1.9595(11) 1.7230(6) 0.7911(3) 0.0252(18) Uani 1 1 d . . . . . H29 H 2.0052 1.7042 0.8239 0.030 Uiso 1 1 calc R U . . . C30 C 1.7735(11) 1.6865(6) 0.7102(4) 0.0284(19) Uani 1 1 d . . . . . H30 H 1.6848 1.6413 0.6853 0.034 Uiso 1 1 calc R U . . . C31 C 1.8280(11) 1.7787(7) 0.6980(4) 0.031(2) Uani 1 1 d . . . . . H31 H 1.7799 1.7961 0.6650 0.037 Uiso 1 1 calc R U . . . C32 C 1.9541(11) 1.8463(6) 0.7343(3) 0.029(2) Uani 1 1 d . . . . . H32 H 1.9944 1.9108 0.7266 0.035 Uiso 1 1 calc R U . . . C33 C 2.0201(10) 1.8185(6) 0.7817(3) 0.0225(17) Uani 1 1 d . . . . . C34 C 2.1574(11) 1.8902(6) 0.8211(3) 0.0254(19) Uani 1 1 d . . . . . C35 C 2.3461(10) 1.9097(6) 0.9057(3) 0.0243(18) Uani 1 1 d . . . . . H35A H 2.4233 1.9554 0.8867 0.029 Uiso 1 1 calc R U . . . H35B H 2.4095 1.8656 0.9205 0.029 Uiso 1 1 calc R U . . . C36 C 2.2968(10) 1.9667(6) 0.9530(3) 0.0235(18) Uani 1 1 d . . . . . C37 C 2.3429(10) 2.0685(6) 0.9611(3) 0.0230(17) Uani 1 1 d . . . . . C38 C 2.4231(11) 2.1262(6) 0.9226(4) 0.0279(19) Uani 1 1 d . . . . . H38 H 2.4445 2.0944 0.8895 0.033 Uiso 1 1 calc R U . . . C39 C 2.4689(12) 2.2245(7) 0.9322(4) 0.034(2) Uani 1 1 d . . . . . H39 H 2.5204 2.2604 0.9057 0.041 Uiso 1 1 calc R U . . . C40 C 2.4413(12) 2.2741(6) 0.9810(4) 0.034(2) Uani 1 1 d . . . . . H40 H 2.4771 2.3431 0.9877 0.041 Uiso 1 1 calc R U . . . C41 C 2.3632(11) 2.2234(6) 1.0188(4) 0.030(2) Uani 1 1 d . . . . . H41 H 2.3451 2.2579 1.0516 0.036 Uiso 1 1 calc R U . . . C42 C 2.3080(10) 2.1194(6) 1.0101(3) 0.0235(18) Uani 1 1 d . . . . . C43 C 2.2233(10) 2.0682(6) 1.0481(3) 0.0217(17) Uani 1 1 d . . . . . C44 C 2.1712(10) 1.9652(6) 1.0392(3) 0.0232(18) Uani 1 1 d . . . . . C45 C 2.0815(10) 1.9081(7) 1.0756(3) 0.0279(19) Uani 1 1 d . . . . . H45 H 2.0535 1.9399 1.1075 0.033 Uiso 1 1 calc R U . . . C46 C 2.0346(11) 1.8089(6) 1.0657(4) 0.029(2) Uani 1 1 d . . . . . H46 H 1.9726 1.7731 1.0904 0.035 Uiso 1 1 calc R U . . . C47 C 2.0772(11) 1.7594(6) 1.0197(4) 0.030(2) Uani 1 1 d . . . . . H47 H 2.0457 1.6904 1.0136 0.036 Uiso 1 1 calc R U . . . C48 C 2.1640(11) 1.8107(6) 0.9836(4) 0.030(2) Uani 1 1 d . . . . . H48 H 2.1931 1.7764 0.9528 0.036 Uiso 1 1 calc R U . . . C49 C 2.2116(10) 1.9134(6) 0.9912(3) 0.0208(17) Uani 1 1 d . . . . . C50 C 2.1763(10) 2.1243(6) 1.0967(3) 0.0253(18) Uani 1 1 d . . . . . H50A H 2.1195 2.1722 1.0831 0.030 Uiso 1 1 calc R U . . . H50B H 2.0939 2.0786 1.1141 0.030 Uiso 1 1 calc R U . . . C51 C 2.3608(11) 2.1268(6) 1.1795(3) 0.0261(19) Uani 1 1 d . . . . . C52 C 2.4961(10) 2.1921(6) 1.2235(3) 0.0215(17) Uani 1 1 d . . . . . C53 C 2.5522(11) 2.1499(6) 1.2679(3) 0.0258(18) Uani 1 1 d . . . . . H53 H 2.5075 2.0827 1.2699 0.031 Uiso 1 1 calc R U . . . C54 C 2.6762(12) 2.2096(6) 1.3094(4) 0.030(2) Uani 1 1 d . . . . . H54 H 2.7189 2.1836 1.3401 0.037 Uiso 1 1 calc R U . . . C55 C 2.7349(11) 2.3059(6) 1.3050(3) 0.029(2) Uani 1 1 d . . . . . H55 H 2.8205 2.3455 1.3332 0.035 Uiso 1 1 calc R U . . . C56 C 2.5612(10) 2.2906(6) 1.2229(3) 0.0226(17) Uani 1 1 d . . . . . H56 H 2.5207 2.3184 1.1926 0.027 Uiso 1 1 calc R U . . . C57 C 1.8514(11) 1.5192(6) 0.5720(4) 0.032(2) Uani 1 1 d . . . . . C58 C 0.6517(17) 0.5082(12) 0.4024(6) 0.081(3) Uani 1 1 d . . . . . H58A H 0.7429 0.5680 0.4150 0.121 Uiso 1 1 calc R U . . . H58B H 0.6997 0.4522 0.4009 0.121 Uiso 1 1 calc R U . . . H58C H 0.5686 0.5013 0.4281 0.121 Uiso 1 1 calc R U . . . C59 C 2.2145(13) 1.4858(7) 0.9258(5) 0.042(3) Uani 1 1 d . . . . . C60 C 1.7545(16) 1.5503(12) 0.9117(6) 0.081(3) Uani 1 1 d . . . . . H60A H 1.8782 1.5670 0.9132 0.121 Uiso 1 1 calc R U . . . H60B H 1.7172 1.4912 0.9285 0.121 Uiso 1 1 calc R U . . . H60C H 1.7225 1.6038 0.9320 0.121 Uiso 1 1 calc R U . . . Ag1 Ag 0.76753(9) 0.51241(5) 0.26910(3) 0.0309(2) Uani 1 1 d . . . . . Ag2 Ag 1.77529(9) 1.50179(5) 0.76619(3) 0.0325(2) Uani 1 1 d . . . . . F1 F 1.7747(9) 1.5870(5) 0.5850(3) 0.0661(8) Uani 1 1 d . . . . . F2 F 1.7794(9) 1.4722(5) 0.5228(3) 0.0661(8) Uani 1 1 d . . . . . F3 F 2.0098(9) 1.5672(5) 0.5661(3) 0.0661(8) Uani 1 1 d . . . . . F4 F 2.1726(9) 1.3909(5) 0.9117(3) 0.0661(8) Uani 1 1 d . . . . . F5 F 2.3709(10) 1.5049(5) 0.9556(3) 0.0661(8) Uani 1 1 d . . . . . F6 F 2.1192(9) 1.5082(5) 0.9612(3) 0.0661(8) Uani 1 1 d . . . . . N1 N 0.8467(9) 0.6698(5) 0.2582(3) 0.0290(16) Uani 1 1 d . . . . . N2 N 1.6828(9) 1.3438(5) 0.7627(3) 0.0300(17) Uani 1 1 d . . . . . N3 N 1.8387(9) 1.6558(5) 0.7556(3) 0.0300(17) Uani 1 1 d . . . . . N4 N 2.6781(9) 2.3487(5) 1.2626(3) 0.0275(16) Uani 1 1 d . . . . . O1 O 1.2167(9) 0.9886(5) 0.3168(3) 0.0420(17) Uani 1 1 d . . . . . O2 O 1.2201(7) 0.8665(4) 0.3657(2) 0.0244(12) Uani 1 1 d . . . . . O3 O 1.3044(9) 1.0387(4) 0.6815(3) 0.0379(16) Uani 1 1 d . . . . . O4 O 1.3163(7) 1.1738(4) 0.6420(2) 0.0242(12) Uani 1 1 d . . . . . O5 O 2.2182(9) 1.9718(5) 0.8134(3) 0.0441(18) Uani 1 1 d . . . . . O6 O 2.2021(7) 1.8524(4) 0.8657(2) 0.0249(13) Uani 1 1 d . . . . . O7 O 2.2958(9) 2.0439(4) 1.1822(3) 0.0407(17) Uani 1 1 d . . . . . O8 O 2.3217(7) 2.1755(4) 1.1384(2) 0.0233(12) Uani 1 1 d . . . . . O9 O 1.9478(8) 1.5052(5) 0.6717(3) 0.0373(15) Uani 1 1 d . . . . . O10 O 1.6801(9) 1.3991(6) 0.6258(3) 0.057(2) Uani 1 1 d . . . . . O11 O 1.9446(11) 1.3736(5) 0.6023(3) 0.0503(19) Uani 1 1 d . . . . . O12 O 0.5673(12) 0.5130(7) 0.3471(3) 0.066(2) Uani 1 1 d . . . . . H12A H 0.4933 0.5435 0.3501 0.099 Uiso 1 1 calc R U . . . O13 O 2.0532(9) 1.5061(6) 0.8355(3) 0.0513(19) Uani 1 1 d . . . . . O14 O 2.3535(8) 1.5241(5) 0.8417(2) 0.0343(14) Uani 1 1 d . . . . . O15 O 2.2522(12) 1.6490(5) 0.8901(3) 0.057(2) Uani 1 1 d . . . . . O16 O 1.6870(15) 1.536(2) 0.8640(4) 0.215(12) Uani 1 1 d . . . . . H16 H 1.5860 1.5029 0.8615 0.323 Uiso 1 1 calc R U . . . S1 S 1.8548(3) 1.44031(16) 0.62389(9) 0.0320(5) Uani 1 1 d . . . . . S3 S 2.2169(3) 1.55050(16) 0.86760(9) 0.0297(5) 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 C1 0.030(4) 0.022(4) 0.018(4) 0.002(3) 0.001(3) 0.010(4) C2 0.034(5) 0.029(5) 0.022(4) -0.004(4) -0.002(4) 0.012(4) C3 0.034(5) 0.031(5) 0.020(4) 0.007(4) 0.000(4) 0.009(4) C4 0.036(5) 0.026(5) 0.020(4) 0.000(4) 0.002(4) 0.011(4) C5 0.029(4) 0.014(4) 0.019(4) 0.003(3) 0.004(3) 0.007(3) C6 0.026(4) 0.031(5) 0.020(4) 0.006(4) 0.007(3) 0.007(4) C7 0.021(4) 0.030(5) 0.024(4) 0.001(4) -0.003(3) 0.007(4) C8 0.020(4) 0.020(4) 0.017(4) 0.001(3) -0.006(3) 0.003(3) C9 0.019(4) 0.028(5) 0.024(4) 0.005(4) -0.007(3) 0.002(3) C10 0.031(5) 0.022(4) 0.026(5) 0.008(4) -0.001(4) -0.001(4) C11 0.043(6) 0.031(5) 0.028(5) 0.009(4) 0.000(4) -0.001(4) C12 0.042(6) 0.024(5) 0.040(6) 0.016(4) -0.007(4) -0.002(4) C13 0.034(5) 0.029(5) 0.029(5) 0.002(4) -0.006(4) 0.011(4) C14 0.021(4) 0.024(4) 0.023(4) 0.004(3) -0.009(3) 0.003(3) C15 0.020(4) 0.024(4) 0.020(4) 0.000(3) -0.005(3) 0.007(3) C16 0.024(4) 0.027(4) 0.019(4) 0.004(3) -0.005(3) 0.005(4) C17 0.026(4) 0.036(5) 0.019(4) 0.006(4) 0.002(3) 0.005(4) C18 0.034(5) 0.023(5) 0.027(5) 0.011(4) -0.005(4) -0.005(4) C19 0.037(5) 0.025(5) 0.030(5) 0.010(4) 0.000(4) 0.003(4) C20 0.031(5) 0.028(5) 0.025(5) 0.005(4) 0.000(4) 0.009(4) C21 0.022(4) 0.026(4) 0.017(4) 0.005(3) -0.007(3) 0.009(3) C22 0.023(4) 0.032(5) 0.022(4) -0.002(4) -0.002(3) 0.010(4) C23 0.024(4) 0.026(5) 0.019(4) 0.001(3) 0.003(3) 0.004(4) C24 0.025(4) 0.025(4) 0.016(4) -0.001(3) 0.004(3) 0.007(4) C25 0.038(5) 0.018(4) 0.028(5) 0.007(4) 0.005(4) 0.011(4) C26 0.033(5) 0.033(5) 0.021(4) 0.004(4) -0.002(4) 0.012(4) C27 0.032(5) 0.032(5) 0.017(4) 0.000(4) -0.004(4) 0.000(4) C28 0.031(5) 0.025(5) 0.023(4) 0.009(4) 0.002(4) 0.005(4) C29 0.028(5) 0.027(5) 0.018(4) 0.002(3) 0.002(3) 0.006(4) C30 0.024(4) 0.031(5) 0.026(5) -0.006(4) -0.002(4) 0.008(4) C31 0.036(5) 0.034(5) 0.024(5) 0.005(4) -0.003(4) 0.014(4) C32 0.038(5) 0.027(5) 0.022(4) 0.002(4) -0.001(4) 0.011(4) C33 0.027(4) 0.021(4) 0.018(4) -0.002(3) 0.000(3) 0.008(3) C34 0.029(5) 0.031(5) 0.018(4) 0.004(4) 0.006(3) 0.011(4) C35 0.020(4) 0.029(5) 0.022(4) -0.001(4) -0.001(3) 0.007(3) C36 0.020(4) 0.029(5) 0.019(4) 0.000(3) -0.005(3) 0.006(3) C37 0.020(4) 0.024(4) 0.021(4) 0.004(3) -0.006(3) 0.003(3) C38 0.025(4) 0.030(5) 0.024(4) 0.006(4) -0.003(4) 0.002(4) C39 0.037(5) 0.031(5) 0.026(5) 0.009(4) -0.004(4) -0.005(4) C40 0.038(5) 0.021(5) 0.038(5) 0.011(4) -0.008(4) 0.000(4) C41 0.035(5) 0.028(5) 0.023(4) 0.001(4) -0.007(4) 0.008(4) C42 0.019(4) 0.022(4) 0.023(4) 0.004(3) -0.011(3) 0.000(3) C43 0.018(4) 0.025(4) 0.020(4) 0.000(3) -0.005(3) 0.006(3) C44 0.020(4) 0.026(4) 0.019(4) 0.002(3) -0.008(3) 0.001(3) C45 0.023(4) 0.039(5) 0.020(4) 0.005(4) 0.001(3) 0.006(4) C46 0.035(5) 0.021(4) 0.025(5) 0.009(4) -0.003(4) -0.002(4) C47 0.031(5) 0.024(5) 0.031(5) 0.011(4) -0.001(4) 0.001(4) C48 0.029(5) 0.031(5) 0.028(5) 0.002(4) -0.006(4) 0.010(4) C49 0.019(4) 0.022(4) 0.019(4) 0.006(3) -0.008(3) 0.003(3) C50 0.021(4) 0.029(5) 0.025(4) -0.002(4) -0.002(3) 0.009(4) C51 0.028(5) 0.028(5) 0.021(4) -0.001(4) 0.003(4) 0.007(4) C52 0.029(4) 0.019(4) 0.015(4) 0.001(3) 0.003(3) 0.004(3) C53 0.035(5) 0.015(4) 0.028(5) 0.008(3) 0.002(4) 0.007(4) C54 0.037(5) 0.027(5) 0.025(5) 0.002(4) -0.002(4) 0.009(4) C55 0.030(5) 0.031(5) 0.017(4) 0.000(4) -0.006(4) 0.000(4) C56 0.028(4) 0.020(4) 0.020(4) 0.005(3) 0.003(3) 0.006(3) C57 0.027(5) 0.020(4) 0.044(6) -0.007(4) -0.001(4) 0.007(4) C58 0.050(5) 0.119(9) 0.068(7) -0.036(6) 0.008(5) 0.033(6) C59 0.039(6) 0.025(5) 0.057(7) -0.011(4) 0.022(5) 0.000(4) C60 0.050(5) 0.119(9) 0.068(7) -0.036(6) 0.008(5) 0.033(6) Ag1 0.0403(4) 0.0201(4) 0.0268(4) 0.0049(3) -0.0004(3) -0.0001(3) Ag2 0.0382(4) 0.0229(4) 0.0296(4) 0.0031(3) 0.0004(3) -0.0017(3) F1 0.078(2) 0.0694(19) 0.0545(17) 0.0301(15) 0.0087(15) 0.0171(16) F2 0.078(2) 0.0694(19) 0.0545(17) 0.0301(15) 0.0087(15) 0.0171(16) F3 0.078(2) 0.0694(19) 0.0545(17) 0.0301(15) 0.0087(15) 0.0171(16) F4 0.078(2) 0.0694(19) 0.0545(17) 0.0301(15) 0.0087(15) 0.0171(16) F5 0.078(2) 0.0694(19) 0.0545(17) 0.0301(15) 0.0087(15) 0.0171(16) F6 0.078(2) 0.0694(19) 0.0545(17) 0.0301(15) 0.0087(15) 0.0171(16) N1 0.034(4) 0.027(4) 0.024(4) 0.005(3) 0.000(3) 0.005(3) N2 0.033(4) 0.019(4) 0.031(4) 0.005(3) -0.002(3) -0.003(3) N3 0.031(4) 0.030(4) 0.024(4) 0.001(3) 0.000(3) 0.003(3) N4 0.031(4) 0.020(4) 0.027(4) 0.004(3) -0.003(3) 0.001(3) O1 0.055(4) 0.026(4) 0.035(4) 0.011(3) -0.011(3) -0.002(3) O2 0.028(3) 0.024(3) 0.021(3) 0.005(2) 0.001(2) 0.008(2) O3 0.051(4) 0.022(4) 0.030(3) 0.005(3) -0.010(3) -0.004(3) O4 0.032(3) 0.019(3) 0.019(3) 0.002(2) -0.001(2) 0.004(2) O5 0.059(5) 0.026(4) 0.035(4) 0.011(3) -0.015(3) -0.004(3) O6 0.029(3) 0.025(3) 0.018(3) 0.004(2) -0.001(2) 0.005(2) O7 0.054(4) 0.022(4) 0.031(4) 0.006(3) -0.011(3) -0.009(3) O8 0.027(3) 0.019(3) 0.021(3) 0.001(2) 0.000(2) 0.003(2) O9 0.040(4) 0.040(4) 0.027(3) 0.004(3) -0.002(3) 0.005(3) O10 0.037(4) 0.079(6) 0.055(5) 0.040(4) 0.006(3) 0.002(4) O11 0.084(6) 0.034(4) 0.040(4) 0.006(3) 0.011(4) 0.029(4) O12 0.082(7) 0.074(6) 0.046(5) 0.011(4) 0.019(4) 0.022(5) O13 0.030(4) 0.073(5) 0.044(4) 0.015(4) -0.007(3) 0.003(4) O14 0.034(3) 0.042(4) 0.030(3) 0.010(3) 0.008(3) 0.013(3) O15 0.102(7) 0.032(4) 0.043(4) 0.004(3) 0.009(4) 0.031(4) O16 0.072(8) 0.57(4) 0.038(6) 0.028(12) 0.011(6) 0.146(15) S1 0.0373(13) 0.0264(12) 0.0271(12) 0.0069(9) -0.0006(10) 0.0000(10) S3 0.0327(12) 0.0281(12) 0.0265(11) 0.0059(9) 0.0008(9) 0.0059(9) _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 C1 N1 1.344(11) . ? C1 C5 1.388(11) . ? C1 H1 0.9500 . ? C2 N1 1.352(11) . ? C2 C3 1.376(13) . ? C2 H2 0.9500 . ? C3 C4 1.381(12) . ? C3 H3 0.9500 . ? C4 C5 1.376(12) . ? C4 H4 0.9500 . ? C5 C6 1.495(12) . ? C6 O1 1.199(11) . ? C6 O2 1.331(10) . ? C7 O2 1.463(10) . ? C7 C8 1.518(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C21 1.405(12) . ? C8 C9 1.407(12) . ? C9 C10 1.432(12) . ? C9 C14 1.437(12) . ? C10 C11 1.355(13) . ? C10 H10 0.9500 . ? C11 C12 1.425(14) . ? C11 H11 0.9500 . ? C12 C13 1.352(13) . ? C12 H12 0.9500 . ? C13 C14 1.436(12) . ? C13 H13 0.9500 . ? C14 C15 1.396(12) . ? C15 C16 1.417(12) . ? C15 C22 1.514(11) . ? C16 C17 1.427(12) . ? C16 C21 1.450(12) . ? C17 C18 1.357(12) . ? C17 H17 0.9500 . ? C18 C19 1.389(13) . ? C18 H18 0.9500 . ? C19 C20 1.368(12) . ? C19 H19 0.9500 . ? C20 C21 1.420(12) . ? C20 H20 0.9500 . ? C22 O4 1.467(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O3 1.182(10) . ? C23 O4 1.353(10) . ? C23 C24 1.504(12) . ? C24 C28 1.378(12) . ? C24 C25 1.387(12) . ? C25 C26 1.384(12) . ? C25 H25 0.9500 . ? C26 C27 1.371(13) . ? C26 H26 0.9500 . ? C27 N2 1.368(11) . ? C27 H27 0.9500 . ? C28 N2 1.336(11) . ? C28 H28 0.9500 . ? C29 N3 1.349(11) . ? C29 C33 1.390(12) . ? C29 H29 0.9500 . ? C30 N3 1.352(12) . ? C30 C31 1.365(13) . ? C30 H30 0.9500 . ? C31 C32 1.383(13) . ? C31 H31 0.9500 . ? C32 C33 1.376(12) . ? C32 H32 0.9500 . ? C33 C34 1.492(12) . ? C34 O5 1.199(11) . ? C34 O6 1.332(10) . ? C35 O6 1.456(10) . ? C35 C36 1.507(11) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.399(12) . ? C36 C49 1.418(12) . ? C37 C38 1.438(12) . ? C37 C42 1.442(12) . ? C38 C39 1.354(13) . ? C38 H38 0.9500 . ? C39 C40 1.403(14) . ? C39 H39 0.9500 . ? C40 C41 1.366(13) . ? C40 H40 0.9500 . ? C41 C42 1.431(12) . ? C41 H41 0.9500 . ? C42 C43 1.398(12) . ? C43 C44 1.417(12) . ? C43 C50 1.514(11) . ? C44 C45 1.426(12) . ? C44 C49 1.448(12) . ? C45 C46 1.365(12) . ? C45 H45 0.9500 . ? C46 C47 1.402(13) . ? C46 H46 0.9500 . ? C47 C48 1.368(13) . ? C47 H47 0.9500 . ? C48 C49 1.414(12) . ? C48 H48 0.9500 . ? C50 O8 1.463(10) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O7 1.189(11) . ? C51 O8 1.347(10) . ? C51 C52 1.508(12) . ? C52 C56 1.384(11) . ? C52 C53 1.397(12) . ? C53 C54 1.397(12) . ? C53 H53 0.9500 . ? C54 C55 1.366(13) . ? C54 H54 0.9500 . ? C55 N4 1.365(11) . ? C55 H55 0.9500 . ? C56 N4 1.336(11) . ? C56 H56 0.9500 . ? C57 F2 1.318(11) . ? C57 F1 1.319(11) . ? C57 F3 1.344(11) . ? C57 S1 1.804(10) . ? C58 O12 1.476(16) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 F6 1.307(11) . ? C59 F4 1.316(12) . ? C59 F5 1.353(13) . ? C59 S3 1.794(12) . ? C60 O16 1.217(16) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? Ag1 N1 2.244(7) . ? Ag1 N4 2.262(7) 1_334 ? Ag2 N3 2.192(7) . ? Ag2 N2 2.193(7) . ? N4 Ag1 2.262(7) 1_776 ? O9 S1 1.430(7) . ? O10 S1 1.418(7) . ? O11 S1 1.444(7) . ? O12 H12A 0.8400 . ? O13 S3 1.435(7) . ? O14 S3 1.464(6) . ? O15 S3 1.408(7) . ? O16 H16 0.8400 . ? 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 C1 C5 123.7(7) . . ? N1 C1 H1 118.1 . . ? C5 C1 H1 118.1 . . ? N1 C2 C3 123.2(8) . . ? N1 C2 H2 118.4 . . ? C3 C2 H2 118.4 . . ? C2 C3 C4 119.8(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 118.1(8) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C4 C5 C1 119.0(8) . . ? C4 C5 C6 119.1(7) . . ? C1 C5 C6 121.9(7) . . ? O1 C6 O2 124.3(8) . . ? O1 C6 C5 123.6(8) . . ? O2 C6 C5 112.1(7) . . ? O2 C7 C8 113.6(6) . . ? O2 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? O2 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C21 C8 C9 120.7(7) . . ? C21 C8 C7 117.8(7) . . ? C9 C8 C7 121.3(7) . . ? C8 C9 C10 123.0(8) . . ? C8 C9 C14 119.1(8) . . ? C10 C9 C14 118.0(8) . . ? C11 C10 C9 121.9(9) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 120.2(9) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.0(9) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 121.9(9) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C9 120.7(8) . . ? C15 C14 C13 121.3(8) . . ? C9 C14 C13 118.0(8) . . ? C14 C15 C16 120.6(8) . . ? C14 C15 C22 119.2(7) . . ? C16 C15 C22 120.1(8) . . ? C15 C16 C17 124.1(8) . . ? C15 C16 C21 118.7(7) . . ? C17 C16 C21 117.3(8) . . ? C18 C17 C16 121.7(8) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 121.1(8) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 120.2(8) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 121.4(8) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C8 C21 C20 121.6(8) . . ? C8 C21 C16 120.1(7) . . ? C20 C21 C16 118.3(8) . . ? O4 C22 C15 112.8(6) . . ? O4 C22 H22A 109.0 . . ? C15 C22 H22A 109.0 . . ? O4 C22 H22B 109.0 . . ? C15 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? O3 C23 O4 125.2(8) . . ? O3 C23 C24 124.4(8) . . ? O4 C23 C24 110.4(7) . . ? C28 C24 C25 119.0(8) . . ? C28 C24 C23 123.5(7) . . ? C25 C24 C23 117.5(7) . . ? C26 C25 C24 118.8(8) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C27 C26 C25 118.8(8) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? N2 C27 C26 123.0(8) . . ? N2 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? N2 C28 C24 123.3(8) . . ? N2 C28 H28 118.4 . . ? C24 C28 H28 118.4 . . ? N3 C29 C33 123.1(8) . . ? N3 C29 H29 118.5 . . ? C33 C29 H29 118.5 . . ? N3 C30 C31 123.7(8) . . ? N3 C30 H30 118.1 . . ? C31 C30 H30 118.1 . . ? C30 C31 C32 119.2(8) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 118.7(8) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C29 118.8(8) . . ? C32 C33 C34 119.5(8) . . ? C29 C33 C34 121.6(7) . . ? O5 C34 O6 124.7(8) . . ? O5 C34 C33 123.5(8) . . ? O6 C34 C33 111.7(7) . . ? O6 C35 C36 113.8(6) . . ? O6 C35 H35A 108.8 . . ? C36 C35 H35A 108.8 . . ? O6 C35 H35B 108.8 . . ? C36 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? C37 C36 C49 121.0(8) . . ? C37 C36 C35 121.6(8) . . ? C49 C36 C35 117.3(7) . . ? C36 C37 C38 123.4(8) . . ? C36 C37 C42 119.2(8) . . ? C38 C37 C42 117.4(8) . . ? C39 C38 C37 121.9(8) . . ? C39 C38 H38 119.0 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 120.7(9) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.7 . . ? C41 C40 C39 120.2(8) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 121.4(9) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C43 C42 C41 121.1(8) . . ? C43 C42 C37 120.6(7) . . ? C41 C42 C37 118.3(8) . . ? C42 C43 C44 120.4(8) . . ? C42 C43 C50 119.0(7) . . ? C44 C43 C50 120.4(7) . . ? C43 C44 C45 123.6(8) . . ? C43 C44 C49 119.3(7) . . ? C45 C44 C49 117.0(7) . . ? C46 C45 C44 121.9(8) . . ? C46 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? C45 C46 C47 120.7(8) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C48 C47 C46 119.9(8) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C47 C48 C49 121.6(9) . . ? C47 C48 H48 119.2 . . ? C49 C48 H48 119.2 . . ? C36 C49 C48 121.7(8) . . ? C36 C49 C44 119.4(7) . . ? C48 C49 C44 118.9(8) . . ? O8 C50 C43 113.7(6) . . ? O8 C50 H50A 108.8 . . ? C43 C50 H50A 108.8 . . ? O8 C50 H50B 108.8 . . ? C43 C50 H50B 108.8 . . ? H50A C50 H50B 107.7 . . ? O7 C51 O8 125.4(8) . . ? O7 C51 C52 123.4(8) . . ? O8 C51 C52 111.2(7) . . ? C56 C52 C53 119.3(8) . . ? C56 C52 C51 123.5(7) . . ? C53 C52 C51 117.1(7) . . ? C54 C53 C52 117.8(8) . . ? C54 C53 H53 121.1 . . ? C52 C53 H53 121.1 . . ? C55 C54 C53 118.9(8) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? N4 C55 C54 123.9(8) . . ? N4 C55 H55 118.0 . . ? C54 C55 H55 118.0 . . ? N4 C56 C52 123.4(7) . . ? N4 C56 H56 118.3 . . ? C52 C56 H56 118.3 . . ? F2 C57 F1 108.5(8) . . ? F2 C57 F3 105.8(8) . . ? F1 C57 F3 105.6(8) . . ? F2 C57 S1 113.2(6) . . ? F1 C57 S1 112.2(7) . . ? F3 C57 S1 111.1(6) . . ? O12 C58 H58A 109.5 . . ? O12 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O12 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? F6 C59 F4 109.4(8) . . ? F6 C59 F5 104.4(9) . . ? F4 C59 F5 103.3(9) . . ? F6 C59 S3 114.3(8) . . ? F4 C59 S3 112.9(7) . . ? F5 C59 S3 111.8(7) . . ? O16 C60 H60A 109.5 . . ? O16 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O16 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N1 Ag1 N4 169.3(3) . 1_334 ? N3 Ag2 N2 169.8(3) . . ? C1 N1 C2 116.2(7) . . ? C1 N1 Ag1 123.7(6) . . ? C2 N1 Ag1 119.8(6) . . ? C28 N2 C27 117.0(7) . . ? C28 N2 Ag2 124.6(6) . . ? C27 N2 Ag2 118.3(6) . . ? C29 N3 C30 116.4(8) . . ? C29 N3 Ag2 121.4(6) . . ? C30 N3 Ag2 121.8(6) . . ? C56 N4 C55 116.6(7) . . ? C56 N4 Ag1 125.1(5) . 1_776 ? C55 N4 Ag1 118.0(5) . 1_776 ? C6 O2 C7 117.8(6) . . ? C23 O4 C22 116.6(6) . . ? C34 O6 C35 118.6(7) . . ? C51 O8 C50 116.7(6) . . ? C58 O12 H12A 109.5 . . ? C60 O16 H16 109.5 . . ? O10 S1 O9 115.7(5) . . ? O10 S1 O11 115.4(5) . . ? O9 S1 O11 113.6(5) . . ? O10 S1 C57 103.3(4) . . ? O9 S1 C57 103.2(4) . . ? O11 S1 C57 103.3(4) . . ? O15 S3 O13 117.6(5) . . ? O15 S3 O14 114.9(5) . . ? O13 S3 O14 112.0(4) . . ? O15 S3 C59 105.1(4) . . ? O13 S3 C59 103.4(5) . . ? O14 S3 C59 101.4(4) . . ? 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 N1 C2 C3 C4 0.2(14) . . . . ? C2 C3 C4 C5 -0.1(13) . . . . ? C3 C4 C5 C1 -0.2(12) . . . . ? C3 C4 C5 C6 -179.8(8) . . . . ? N1 C1 C5 C4 0.3(13) . . . . ? N1 C1 C5 C6 179.9(8) . . . . ? C4 C5 C6 O1 1.6(13) . . . . ? C1 C5 C6 O1 -178.1(8) . . . . ? C4 C5 C6 O2 -178.5(7) . . . . ? C1 C5 C6 O2 1.9(11) . . . . ? O2 C7 C8 C21 66.6(9) . . . . ? O2 C7 C8 C9 -118.1(8) . . . . ? C21 C8 C9 C10 -178.1(7) . . . . ? C7 C8 C9 C10 6.8(12) . . . . ? C21 C8 C9 C14 2.9(11) . . . . ? C7 C8 C9 C14 -172.3(7) . . . . ? C8 C9 C10 C11 -178.4(8) . . . . ? C14 C9 C10 C11 0.6(12) . . . . ? C9 C10 C11 C12 1.5(14) . . . . ? C10 C11 C12 C13 -2.2(14) . . . . ? C11 C12 C13 C14 0.7(14) . . . . ? C8 C9 C14 C15 -3.2(11) . . . . ? C10 C9 C14 C15 177.7(7) . . . . ? C8 C9 C14 C13 177.0(7) . . . . ? C10 C9 C14 C13 -2.1(11) . . . . ? C12 C13 C14 C15 -178.4(8) . . . . ? C12 C13 C14 C9 1.4(12) . . . . ? C9 C14 C15 C16 0.9(12) . . . . ? C13 C14 C15 C16 -179.3(7) . . . . ? C9 C14 C15 C22 -176.0(7) . . . . ? C13 C14 C15 C22 3.8(11) . . . . ? C14 C15 C16 C17 -178.9(7) . . . . ? C22 C15 C16 C17 -2.1(12) . . . . ? C14 C15 C16 C21 1.7(11) . . . . ? C22 C15 C16 C21 178.5(7) . . . . ? C15 C16 C17 C18 179.8(8) . . . . ? C21 C16 C17 C18 -0.7(12) . . . . ? C16 C17 C18 C19 1.1(13) . . . . ? C17 C18 C19 C20 0.2(14) . . . . ? C18 C19 C20 C21 -1.8(13) . . . . ? C9 C8 C21 C20 179.0(7) . . . . ? C7 C8 C21 C20 -5.6(11) . . . . ? C9 C8 C21 C16 -0.3(11) . . . . ? C7 C8 C21 C16 175.0(7) . . . . ? C19 C20 C21 C8 -177.3(8) . . . . ? C19 C20 C21 C16 2.1(12) . . . . ? C15 C16 C21 C8 -2.0(11) . . . . ? C17 C16 C21 C8 178.6(7) . . . . ? C15 C16 C21 C20 178.6(7) . . . . ? C17 C16 C21 C20 -0.8(11) . . . . ? C14 C15 C22 O4 -70.5(9) . . . . ? C16 C15 C22 O4 112.7(8) . . . . ? O3 C23 C24 C28 -179.9(9) . . . . ? O4 C23 C24 C28 -0.9(11) . . . . ? O3 C23 C24 C25 -0.6(13) . . . . ? O4 C23 C24 C25 178.3(7) . . . . ? C28 C24 C25 C26 -0.1(12) . . . . ? C23 C24 C25 C26 -179.4(8) . . . . ? C24 C25 C26 C27 1.2(13) . . . . ? C25 C26 C27 N2 -0.7(14) . . . . ? C25 C24 C28 N2 -1.6(13) . . . . ? C23 C24 C28 N2 177.7(8) . . . . ? N3 C30 C31 C32 -1.6(14) . . . . ? C30 C31 C32 C33 -0.3(13) . . . . ? C31 C32 C33 C29 1.0(13) . . . . ? C31 C32 C33 C34 179.4(8) . . . . ? N3 C29 C33 C32 0.2(13) . . . . ? N3 C29 C33 C34 -178.2(8) . . . . ? C32 C33 C34 O5 -1.8(13) . . . . ? C29 C33 C34 O5 176.6(9) . . . . ? C32 C33 C34 O6 177.7(7) . . . . ? C29 C33 C34 O6 -3.9(11) . . . . ? O6 C35 C36 C37 -114.5(8) . . . . ? O6 C35 C36 C49 69.6(9) . . . . ? C49 C36 C37 C38 -177.3(7) . . . . ? C35 C36 C37 C38 6.9(12) . . . . ? C49 C36 C37 C42 2.2(12) . . . . ? C35 C36 C37 C42 -173.5(7) . . . . ? C36 C37 C38 C39 -178.7(8) . . . . ? C42 C37 C38 C39 1.7(12) . . . . ? C37 C38 C39 C40 0.8(14) . . . . ? C38 C39 C40 C41 -1.8(14) . . . . ? C39 C40 C41 C42 0.2(14) . . . . ? C40 C41 C42 C43 -177.9(8) . . . . ? C40 C41 C42 C37 2.4(12) . . . . ? C36 C37 C42 C43 -2.5(11) . . . . ? C38 C37 C42 C43 177.0(7) . . . . ? C36 C37 C42 C41 177.2(7) . . . . ? C38 C37 C42 C41 -3.3(11) . . . . ? C41 C42 C43 C44 -179.3(7) . . . . ? C37 C42 C43 C44 0.4(12) . . . . ? C41 C42 C43 C50 5.3(11) . . . . ? C37 C42 C43 C50 -175.0(7) . . . . ? C42 C43 C44 C45 -178.8(7) . . . . ? C50 C43 C44 C45 -3.4(12) . . . . ? C42 C43 C44 C49 2.0(11) . . . . ? C50 C43 C44 C49 177.4(7) . . . . ? C43 C44 C45 C46 -179.5(8) . . . . ? C49 C44 C45 C46 -0.3(12) . . . . ? C44 C45 C46 C47 1.5(13) . . . . ? C45 C46 C47 C48 -1.1(13) . . . . ? C46 C47 C48 C49 -0.5(13) . . . . ? C37 C36 C49 C48 179.9(7) . . . . ? C35 C36 C49 C48 -4.2(11) . . . . ? C37 C36 C49 C44 0.2(11) . . . . ? C35 C36 C49 C44 176.1(7) . . . . ? C47 C48 C49 C36 -178.0(8) . . . . ? C47 C48 C49 C44 1.8(12) . . . . ? C43 C44 C49 C36 -2.4(11) . . . . ? C45 C44 C49 C36 178.4(7) . . . . ? C43 C44 C49 C48 177.9(7) . . . . ? C45 C44 C49 C48 -1.3(11) . . . . ? C42 C43 C50 O8 -72.4(9) . . . . ? C44 C43 C50 O8 112.1(8) . . . . ? O7 C51 C52 C56 -174.0(9) . . . . ? O8 C51 C52 C56 4.2(11) . . . . ? O7 C51 C52 C53 3.6(13) . . . . ? O8 C51 C52 C53 -178.2(7) . . . . ? C56 C52 C53 C54 -1.6(12) . . . . ? C51 C52 C53 C54 -179.3(8) . . . . ? C52 C53 C54 C55 0.8(13) . . . . ? C53 C54 C55 N4 1.0(14) . . . . ? C53 C52 C56 N4 0.8(13) . . . . ? C51 C52 C56 N4 178.3(8) . . . . ? C5 C1 N1 C2 -0.2(12) . . . . ? C5 C1 N1 Ag1 173.6(6) . . . . ? C3 C2 N1 C1 -0.1(13) . . . . ? C3 C2 N1 Ag1 -174.1(7) . . . . ? C24 C28 N2 C27 2.1(13) . . . . ? C24 C28 N2 Ag2 -174.0(6) . . . . ? C26 C27 N2 C28 -1.0(13) . . . . ? C26 C27 N2 Ag2 175.5(7) . . . . ? C33 C29 N3 C30 -2.0(12) . . . . ? C33 C29 N3 Ag2 170.7(6) . . . . ? C31 C30 N3 C29 2.7(13) . . . . ? C31 C30 N3 Ag2 -170.0(7) . . . . ? C52 C56 N4 C55 0.9(12) . . . . ? C52 C56 N4 Ag1 -172.6(6) . . . 1_776 ? C54 C55 N4 C56 -1.8(13) . . . . ? C54 C55 N4 Ag1 172.2(7) . . . 1_776 ? O1 C6 O2 C7 -3.5(12) . . . . ? C5 C6 O2 C7 176.5(6) . . . . ? C8 C7 O2 C6 92.6(8) . . . . ? O3 C23 O4 C22 6.4(12) . . . . ? C24 C23 O4 C22 -172.6(6) . . . . ? C15 C22 O4 C23 -90.4(9) . . . . ? O5 C34 O6 C35 -6.4(12) . . . . ? C33 C34 O6 C35 174.0(6) . . . . ? C36 C35 O6 C34 95.2(9) . . . . ? O7 C51 O8 C50 6.2(12) . . . . ? C52 C51 O8 C50 -172.0(6) . . . . ? C43 C50 O8 C51 -91.1(9) . . . . ? F2 C57 S1 O10 -63.1(8) . . . . ? F1 C57 S1 O10 60.1(8) . . . . ? F3 C57 S1 O10 178.1(7) . . . . ? F2 C57 S1 O9 176.0(7) . . . . ? F1 C57 S1 O9 -60.8(7) . . . . ? F3 C57 S1 O9 57.2(7) . . . . ? F2 C57 S1 O11 57.5(8) . . . . ? F1 C57 S1 O11 -179.3(7) . . . . ? F3 C57 S1 O11 -61.4(7) . . . . ? F6 C59 S3 O15 50.3(9) . . . . ? F4 C59 S3 O15 176.1(8) . . . . ? F5 C59 S3 O15 -68.0(8) . . . . ? F6 C59 S3 O13 -73.5(8) . . . . ? F4 C59 S3 O13 52.3(8) . . . . ? F5 C59 S3 O13 168.2(7) . . . . ? F6 C59 S3 O14 170.3(7) . . . . ? F4 C59 S3 O14 -63.9(8) . . . . ? F5 C59 S3 O14 52.0(7) . . . . ? 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 C1 H1 O11 0.95 2.38 3.288(11) 160.8 2_876 C2 H2 O14 0.95 2.49 3.200(11) 132.0 2_876 C27 H27 O13 0.95 2.61 3.324(12) 132.1 . C28 H28 O10 0.95 2.44 3.150(11) 131.1 . C30 H30 O12 0.95 2.60 3.498(13) 157.2 2_776 C55 H55 O9 0.95 2.51 3.202(11) 129.8 2_:97 C56 H56 O14 0.95 2.52 3.220(10) 130.5 2_:97 C58 H58A O11 0.98 2.60 3.348(17) 133.7 2_876 C58 H58B F3 0.98 2.53 3.275(15) 133.0 2_876 C60 H60A F6 0.98 2.56 3.328(15) 135.1 . O12 H12A O10 0.84 1.94 2.758(12) 165.6 2_776 O16 H16 O14 0.84 2.02 2.692(12) 135.9 1_455 _refine_diff_density_max 1.774 _refine_diff_density_min -1.804 _refine_diff_density_rms 0.143 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL Complex2 CELL 0.71073 8.2252 14.3623 24.7106 96.204 96.652 104.577 ZERR 2.00 0.0016 0.0029 0.0049 0.030 0.030 0.030 LATT 1 SFAC C H AG F N O S UNIT 120 96 4 12 8 32 4 MERG 2 OMIT 0.00 50.00 TWIN EQIV $1 -x+3, -y+2, -z+1 HTAB C1 O11_$1 HTAB C2 O14_$1 HTAB C27 O13 HTAB C28 O10 EQIV $2 -x+2, -y+2, -z+1 HTAB C30 O12_$2 EQIV $3 -x+5, -y+4, -z+2 HTAB C55 O9_$3 HTAB C56 O14_$3 HTAB C58 O11_$1 HTAB C58 F3_$1 HTAB C60 F6 HTAB O12 O10_$2 EQIV $4 x-1, y, z HTAB O16 O14_$4 EADP F1 F2 F3 F4 F5 F6 EADP C58 C60 OMIT 0 3 0 OMIT 0 -2 6 OMIT 2 -3 20 OMIT -2 0 18 OMIT 4 -1 2 OMIT 2 -6 20 OMIT 0 10 6 OMIT 4 -3 8 OMIT 3 -10 2 OMIT 4 -6 14 FMAP 2 PLAN 5 SIZE 0.120 0.180 0.220 ACTA BOND $H CONF L.S. 20 TEMP -123.10 WGHT 0.071500 52.209301 BASF -0.81914 FVAR 0.10695 C1 1 0.968566 0.737246 0.292771 11.00000 0.02992 0.02158 = 0.01846 0.00195 0.00068 0.01027 AFIX 43 H1 2 1.015955 0.718701 0.325494 11.00000 -1.20000 AFIX 0 C2 1 0.782501 0.699266 0.212211 11.00000 0.03367 0.02949 = 0.02199 -0.00387 -0.00168 0.01204 AFIX 43 H2 2 0.696261 0.653370 0.186861 11.00000 -1.20000 AFIX 0 C3 1 0.836031 0.792554 0.200356 11.00000 0.03379 0.03081 = 0.01988 0.00665 0.00043 0.00867 AFIX 43 H3 2 0.786809 0.809920 0.167532 11.00000 -1.20000 AFIX 0 C4 1 0.961517 0.860875 0.236308 11.00000 0.03588 0.02598 = 0.02035 0.00044 0.00198 0.01139 AFIX 43 H4 2 1.000108 0.925615 0.228774 11.00000 -1.20000 AFIX 0 C5 1 1.029044 0.832501 0.283349 11.00000 0.02857 0.01416 = 0.01914 0.00314 0.00362 0.00747 C6 1 1.164667 0.905249 0.322997 11.00000 0.02585 0.03058 = 0.01971 0.00575 0.00729 0.00735 C7 1 1.360155 0.928477 0.406072 11.00000 0.02116 0.02964 = 0.02416 0.00055 -0.00257 0.00713 AFIX 23 H7A 2 1.431252 0.977692 0.387378 11.00000 -1.20000 H7B 2 1.431898 0.888073 0.420483 11.00000 -1.20000 AFIX 0 C8 1 1.302268 0.980227 0.454091 11.00000 0.01955 0.02009 = 0.01731 0.00090 -0.00643 0.00337 C9 1 1.342534 1.082340 0.464482 11.00000 0.01886 0.02765 = 0.02375 0.00514 -0.00671 0.00218 C10 1 1.423722 1.143753 0.428003 11.00000 0.03135 0.02197 = 0.02582 0.00758 -0.00128 -0.00135 AFIX 43 H10 2 1.449442 1.114814 0.394773 11.00000 -1.20000 AFIX 0 C11 1 1.464888 1.241982 0.439555 11.00000 0.04263 0.03092 = 0.02832 0.00894 -0.00010 -0.00119 AFIX 43 H11 2 1.516180 1.280789 0.414118 11.00000 -1.20000 AFIX 0 C12 1 1.431462 1.287241 0.489750 11.00000 0.04183 0.02410 = 0.04021 0.01590 -0.00742 -0.00227 AFIX 43 H12 2 1.464110 1.356084 0.498323 11.00000 -1.20000 AFIX 0 C13 1 1.353294 1.232215 0.525170 11.00000 0.03377 0.02912 = 0.02882 0.00215 -0.00616 0.01066 AFIX 43 H13 2 1.330699 1.263437 0.558270 11.00000 -1.20000 AFIX 0 C14 1 1.303436 1.127917 0.514192 11.00000 0.02067 0.02363 = 0.02263 0.00360 -0.00896 0.00302 C15 1 1.218988 1.072070 0.550458 11.00000 0.01984 0.02433 = 0.01976 -0.00037 -0.00459 0.00661 C16 1 1.172168 0.969216 0.539352 11.00000 0.02379 0.02676 = 0.01870 0.00389 -0.00516 0.00496 C17 1 1.083225 0.907058 0.573790 11.00000 0.02592 0.03595 = 0.01871 0.00561 0.00164 0.00485 AFIX 43 H17 2 1.052751 0.935170 0.606398 11.00000 -1.20000 AFIX 0 C18 1 1.041050 0.808849 0.561171 11.00000 0.03393 0.02288 = 0.02693 0.01145 -0.00479 -0.00510 AFIX 43 H18 2 0.980068 0.769668 0.584700 11.00000 -1.20000 AFIX 0 C19 1 1.085620 0.764660 0.514388 11.00000 0.03692 0.02486 = 0.03018 0.00955 0.00048 0.00314 AFIX 43 H19 2 1.054680 0.695786 0.506139 11.00000 -1.20000 AFIX 0 C20 1 1.173926 0.820011 0.480159 11.00000 0.03089 0.02760 = 0.02548 0.00492 -0.00048 0.00937 AFIX 43 H20 2 1.206461 0.788798 0.448904 11.00000 -1.20000 AFIX 0 C21 1 1.217973 0.923152 0.490370 11.00000 0.02225 0.02561 = 0.01741 0.00541 -0.00662 0.00905 C22 1 1.169553 1.122594 0.600500 11.00000 0.02272 0.03249 = 0.02249 -0.00179 -0.00217 0.01034 AFIX 23 H22A 2 1.108219 1.169796 0.588687 11.00000 -1.20000 H22B 2 1.090953 1.073776 0.617345 11.00000 -1.20000 AFIX 0 C23 1 1.363240 1.122543 0.680997 11.00000 0.02406 0.02628 = 0.01912 0.00116 0.00342 0.00420 C24 1 1.499407 1.187760 0.724480 11.00000 0.02519 0.02520 = 0.01583 -0.00100 0.00356 0.00710 C25 1 1.558394 1.146545 0.768367 11.00000 0.03844 0.01770 = 0.02791 0.00677 0.00504 0.01103 AFIX 43 H25 2 1.514295 1.079380 0.770325 11.00000 -1.20000 AFIX 0 C26 1 1.682632 1.204977 0.809261 11.00000 0.03328 0.03260 = 0.02061 0.00352 -0.00247 0.01178 AFIX 43 H26 2 1.726855 1.178374 0.839423 11.00000 -1.20000 AFIX 0 C27 1 1.740749 1.301913 0.805477 11.00000 0.03228 0.03240 = 0.01744 0.00014 -0.00401 0.00018 AFIX 43 H27 2 1.825138 1.341833 0.833864 11.00000 -1.20000 AFIX 0 C28 1 1.566002 1.285457 0.723052 11.00000 0.03069 0.02543 = 0.02260 0.00950 0.00168 0.00545 AFIX 43 H28 2 1.526915 1.312668 0.692350 11.00000 -1.20000 AFIX 0 C29 1 1.959461 1.723005 0.791055 11.00000 0.02848 0.02750 = 0.01836 0.00185 0.00213 0.00646 AFIX 43 H29 2 2.005224 1.704222 0.823942 11.00000 -1.20000 AFIX 0 C30 1 1.773529 1.686455 0.710159 11.00000 0.02426 0.03130 = 0.02621 -0.00551 -0.00199 0.00756 AFIX 43 H30 2 1.684819 1.641295 0.685289 11.00000 -1.20000 AFIX 0 C31 1 1.827998 1.778661 0.698011 11.00000 0.03557 0.03438 = 0.02422 0.00499 -0.00321 0.01400 AFIX 43 H31 2 1.779886 1.796135 0.665050 11.00000 -1.20000 AFIX 0 C32 1 1.954112 1.846343 0.734286 11.00000 0.03768 0.02745 = 0.02248 0.00179 -0.00104 0.01130 AFIX 43 H32 2 1.994420 1.910846 0.726583 11.00000 -1.20000 AFIX 0 C33 1 2.020082 1.818460 0.781749 11.00000 0.02741 0.02086 = 0.01817 -0.00207 0.00031 0.00778 C34 1 2.157352 1.890151 0.821144 11.00000 0.02913 0.03133 = 0.01819 0.00380 0.00609 0.01116 C35 1 2.346080 1.909690 0.905697 11.00000 0.01981 0.02862 = 0.02248 -0.00066 -0.00146 0.00663 AFIX 23 H35A 2 2.423337 1.955400 0.886726 11.00000 -1.20000 H35B 2 2.409524 1.865577 0.920516 11.00000 -1.20000 AFIX 0 C36 1 2.296826 1.966739 0.952981 11.00000 0.01971 0.02890 = 0.01904 0.00034 -0.00508 0.00609 C37 1 2.342855 2.068457 0.961068 11.00000 0.02026 0.02409 = 0.02097 0.00352 -0.00562 0.00294 C38 1 2.423072 2.126196 0.922603 11.00000 0.02497 0.03018 = 0.02434 0.00553 -0.00291 0.00188 AFIX 43 H38 2 2.444511 2.094413 0.889483 11.00000 -1.20000 AFIX 0 C39 1 2.468935 2.224540 0.932215 11.00000 0.03657 0.03055 = 0.02582 0.00856 -0.00370 -0.00457 AFIX 43 H39 2 2.520357 2.260413 0.905663 11.00000 -1.20000 AFIX 0 C40 1 2.441333 2.274061 0.980981 11.00000 0.03795 0.02127 = 0.03764 0.01050 -0.00802 -0.00022 AFIX 43 H40 2 2.477105 2.343057 0.987723 11.00000 -1.20000 AFIX 0 C41 1 2.363188 2.223399 1.018805 11.00000 0.03500 0.02804 = 0.02342 0.00106 -0.00655 0.00789 AFIX 43 H41 2 2.345063 2.257924 1.051582 11.00000 -1.20000 AFIX 0 C42 1 2.308040 2.119422 1.010109 11.00000 0.01879 0.02227 = 0.02310 0.00378 -0.01137 0.00027 C43 1 2.223289 2.068195 1.048139 11.00000 0.01821 0.02484 = 0.01988 0.00015 -0.00461 0.00625 C44 1 2.171161 1.965222 1.039231 11.00000 0.01974 0.02570 = 0.01855 0.00216 -0.00780 0.00105 C45 1 2.081451 1.908075 1.075563 11.00000 0.02346 0.03860 = 0.02043 0.00502 0.00141 0.00650 AFIX 43 H45 2 2.053472 1.939906 1.107518 11.00000 -1.20000 AFIX 0 C46 1 2.034628 1.808940 1.065740 11.00000 0.03547 0.02052 = 0.02491 0.00916 -0.00276 -0.00197 AFIX 43 H46 2 1.972564 1.773120 1.090352 11.00000 -1.20000 AFIX 0 C47 1 2.077165 1.759421 1.019711 11.00000 0.03135 0.02394 = 0.03085 0.01135 -0.00098 0.00079 AFIX 43 H47 2 2.045731 1.690378 1.013574 11.00000 -1.20000 AFIX 0 C48 1 2.164006 1.810663 0.983641 11.00000 0.02854 0.03135 = 0.02787 0.00215 -0.00573 0.00981 AFIX 43 H48 2 2.193061 1.776374 0.952752 11.00000 -1.20000 AFIX 0 C49 1 2.211577 1.913422 0.991215 11.00000 0.01884 0.02172 = 0.01862 0.00594 -0.00840 0.00341 C50 1 2.176349 2.124266 1.096669 11.00000 0.02115 0.02872 = 0.02456 -0.00244 -0.00189 0.00914 AFIX 23 H50A 2 2.119534 2.172173 1.083074 11.00000 -1.20000 H50B 2 2.093866 2.078552 1.114052 11.00000 -1.20000 AFIX 0 C51 1 2.360805 2.126778 1.179506 11.00000 0.02783 0.02761 = 0.02130 -0.00056 0.00286 0.00676 C52 1 2.496055 2.192067 1.223519 11.00000 0.02855 0.01934 = 0.01471 0.00052 0.00305 0.00396 C53 1 2.552179 2.149867 1.267910 11.00000 0.03516 0.01499 = 0.02807 0.00832 0.00243 0.00682 AFIX 43 H53 2 2.507508 2.082744 1.269856 11.00000 -1.20000 AFIX 0 C54 1 2.676155 2.209572 1.309365 11.00000 0.03686 0.02724 = 0.02521 0.00206 -0.00241 0.00881 AFIX 43 H54 2 2.718861 2.183628 1.340052 11.00000 -1.20000 AFIX 0 C55 1 2.734920 2.305908 1.305014 11.00000 0.03045 0.03104 = 0.01690 -0.00038 -0.00637 -0.00039 AFIX 43 H55 2 2.820478 2.345497 1.333179 11.00000 -1.20000 AFIX 0 C56 1 2.561182 2.290608 1.222889 11.00000 0.02805 0.02010 = 0.01972 0.00499 0.00268 0.00614 AFIX 43 H56 2 2.520695 2.318399 1.192644 11.00000 -1.20000 AFIX 0 C57 1 1.851449 1.519243 0.571982 11.00000 0.02716 0.02015 = 0.04433 -0.00689 -0.00082 0.00730 C58 1 0.651715 0.508247 0.402437 11.00000 0.05002 0.11920 = 0.06769 -0.03561 0.00812 0.03329 AFIX 137 H58A 2 0.742920 0.568005 0.415043 11.00000 -1.50000 H58B 2 0.699657 0.452244 0.400856 11.00000 -1.50000 H58C 2 0.568598 0.501313 0.428132 11.00000 -1.50000 AFIX 0 C59 1 2.214493 1.485811 0.925797 11.00000 0.03919 0.02486 = 0.05654 -0.01136 0.02198 0.00003 C60 1 1.754526 1.550268 0.911749 11.00000 0.05002 0.11920 = 0.06769 -0.03561 0.00812 0.03329 AFIX 137 H60A 2 1.878196 1.566973 0.913199 11.00000 -1.50000 H60B 2 1.717208 1.491150 0.928490 11.00000 -1.50000 H60C 2 1.722522 1.603817 0.931997 11.00000 -1.50000 AFIX 0 AG1 3 0.767533 0.512408 0.269100 11.00000 0.04035 0.02011 = 0.02676 0.00489 -0.00045 -0.00008 AG2 3 1.775293 1.501794 0.766191 11.00000 0.03817 0.02285 = 0.02964 0.00314 0.00037 -0.00174 F1 4 1.774654 1.587029 0.584980 11.00000 0.07761 0.06941 = 0.05453 0.03009 0.00873 0.01706 F2 4 1.779356 1.472250 0.522819 11.00000 0.07761 0.06941 = 0.05453 0.03009 0.00873 0.01706 F3 4 2.009814 1.567196 0.566079 11.00000 0.07761 0.06941 = 0.05453 0.03009 0.00873 0.01706 F4 4 2.172611 1.390932 0.911664 11.00000 0.07761 0.06941 = 0.05453 0.03009 0.00873 0.01706 F5 4 2.370863 1.504930 0.955623 11.00000 0.07761 0.06941 = 0.05453 0.03009 0.00873 0.01706 F6 4 2.119164 1.508177 0.961197 11.00000 0.07761 0.06941 = 0.05453 0.03009 0.00873 0.01706 N1 5 0.846745 0.669752 0.258219 11.00000 0.03381 0.02709 = 0.02373 0.00450 0.00023 0.00508 N2 5 1.682819 1.343814 0.762705 11.00000 0.03290 0.01925 = 0.03067 0.00474 -0.00189 -0.00335 N3 5 1.838671 1.655753 0.755580 11.00000 0.03112 0.02959 = 0.02436 0.00053 -0.00025 0.00250 N4 5 2.678075 2.348656 1.262637 11.00000 0.03072 0.01958 = 0.02749 0.00416 -0.00261 0.00109 O1 6 1.216729 0.988640 0.316784 11.00000 0.05532 0.02574 = 0.03512 0.01134 -0.01125 -0.00168 O2 6 1.220099 0.866524 0.365670 11.00000 0.02828 0.02430 = 0.02079 0.00522 0.00067 0.00778 O3 6 1.304400 1.038679 0.681549 11.00000 0.05112 0.02154 = 0.03016 0.00544 -0.00968 -0.00375 O4 6 1.316311 1.173812 0.642000 11.00000 0.03163 0.01890 = 0.01945 0.00203 -0.00094 0.00440 O5 6 2.218160 1.971810 0.813355 11.00000 0.05946 0.02586 = 0.03484 0.01136 -0.01492 -0.00394 O6 6 2.202109 1.852377 0.865652 11.00000 0.02903 0.02501 = 0.01847 0.00375 -0.00097 0.00520 O7 6 2.295836 2.043889 1.182236 11.00000 0.05425 0.02242 = 0.03127 0.00618 -0.01102 -0.00891 O8 6 2.321673 2.175477 1.138406 11.00000 0.02663 0.01882 = 0.02142 0.00110 0.00032 0.00278 O9 6 1.947803 1.505220 0.671735 11.00000 0.04004 0.03958 = 0.02705 0.00354 -0.00156 0.00465 O10 6 1.680117 1.399114 0.625804 11.00000 0.03693 0.07919 = 0.05467 0.03951 0.00618 0.00166 O11 6 1.944632 1.373633 0.602263 11.00000 0.08439 0.03400 = 0.04039 0.00636 0.01093 0.02921 O12 6 0.567333 0.513033 0.347137 11.00000 0.08151 0.07368 = 0.04649 0.01104 0.01873 0.02155 AFIX 147 H12A 2 0.493298 0.543524 0.350104 11.00000 -1.50000 AFIX 0 O13 6 2.053210 1.506128 0.835542 11.00000 0.02956 0.07329 = 0.04375 0.01454 -0.00666 0.00309 O14 6 2.353467 1.524053 0.841738 11.00000 0.03446 0.04205 = 0.02965 0.00981 0.00768 0.01314 O15 6 2.252226 1.649018 0.890118 11.00000 0.10225 0.03161 = 0.04269 0.00390 0.00869 0.03112 O16 6 1.687017 1.536432 0.864000 11.00000 0.07237 0.56543 = 0.03819 0.02772 0.01147 0.14575 AFIX 147 H16 2 1.586041 1.502938 0.861495 11.00000 -1.50000 AFIX 0 S1 7 1.854839 1.440310 0.623894 11.00000 0.03726 0.02638 = 0.02710 0.00686 -0.00063 0.00002 S3 7 2.216871 1.550500 0.867602 11.00000 0.03272 0.02814 = 0.02652 0.00588 0.00079 0.00591 HKLF 4 REM Complex2 REM R1 = 0.0770 for 7530 Fo > 4sig(Fo) and 0.0814 for all 8275 data REM 780 parameters refined using 0 restraints END WGHT 0.0360 48.9727 REM Highest difference peak 1.774, deepest hole -1.804, 1-sigma level 0.143 Q1 1 1.8335 1.4988 0.6074 11.00000 0.05 1.77 Q2 1 2.1697 1.4963 0.8904 11.00000 0.05 1.51 Q3 1 0.7085 0.5059 0.4312 11.00000 0.05 1.46 Q4 1 2.0366 1.4558 0.9410 11.00000 0.05 1.45 Q5 1 1.6367 1.4977 0.5903 11.00000 0.05 1.24 ; _shelx_res_checksum 90713 # start Validation Reply Form _vrf_THETM01_complex2 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: no diffraction recorded in high angles ; _vrf_PLAT222_complex2 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) ... 10.0 Ratio RESPONSE: H atom attach to O16, which as a large Ueq ; _vrf_PLAT241_complex2 ; PROBLEM: High Ueq as Compared to Neighbors for ..... O16 Check RESPONSE: O atom attach to Ag atom but also doing some H-bonding, the splitting of this atom didn't solve the problem ; _vrf_PLAT112_complex2 ; PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... c/2 Check RESPONSE: No higher symmetry possible ; # end Validation Reply Form ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_AgTriflatediNicoAnthra _database_code_depnum_ccdc_archive 'CCDC 1547594' _audit_update_record ; 2017-07-11 deposited with the CCDC. 2017-07-31 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H20 Ag N2 O4, C F3 O3 S' _chemical_formula_sum 'C29 H20 Ag F3 N2 O7 S' _exptl_crystal_recrystallization_method 'DCM, MeOH' _chemical_melting_point ? _exptl_crystal_description needle _exptl_crystal_colour Yellow _diffrn_ambient_temperature 298(2) _chemical_formula_weight 705.40 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' Ag Ag -0.8971 1.1015 '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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _chemical_absolute_configuration ? loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2703(17) _cell_length_b 12.916(3) _cell_length_c 13.267(3) _cell_angle_alpha 98.584(16) _cell_angle_beta 99.288(16) _cell_angle_gamma 98.638(17) _cell_volume 1360.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 11364 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 25.51 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_F_000 708 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.107 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.891 _shelx_estimated_absorpt_T_min 0.821 _shelx_estimated_absorpt_T_max 0.982 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3436 _exptl_absorpt_correction_T_max 0.6410 _exptl_absorpt_process_details ; Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17323 _diffrn_reflns_av_unetI/netI 0.1273 _diffrn_reflns_av_R_equivalents 0.1894 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.581 _diffrn_reflns_theta_max 25.372 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_point_group_measured_fraction_full 0.993 _reflns_number_total 4893 _reflns_number_gt 2560 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'X-Area (Stoe & Cie, 2009)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2009)' _computing_data_reduction 'X-RED32(Stoe & Cie, 2009)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+2.4033P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4893 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1699 _refine_ls_R_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.2257 _refine_ls_wR_factor_gt 0.1870 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4614(12) 0.4268(8) 0.2338(8) 0.070(3) Uani 1 1 d . . . . . H1 H 0.4305 0.3632 0.2564 0.085 Uiso 1 1 calc R U . . . C2 C 0.6242(13) 0.5917(10) 0.2593(10) 0.087(3) Uani 1 1 d . . . . . H2 H 0.7091 0.6432 0.3009 0.104 Uiso 1 1 calc R U . . . C3 C 0.5485(14) 0.6132(9) 0.1654(10) 0.084(3) Uani 1 1 d . . . . . H3 H 0.5816 0.6774 0.1444 0.101 Uiso 1 1 calc R U . . . C4 C 0.4224(14) 0.5364(9) 0.1041(9) 0.079(3) Uani 1 1 d . . . . . H4 H 0.3673 0.5482 0.0412 0.095 Uiso 1 1 calc R U . . . C5 C 0.3799(12) 0.4422(9) 0.1379(8) 0.072(3) Uani 1 1 d . . . . . C6 C 0.2446(13) 0.3570(9) 0.0715(9) 0.076(3) Uani 1 1 d . . . . . C7 C 0.1171(12) 0.1724(8) 0.0441(8) 0.075(3) Uani 1 1 d . . . . . H7A H 0.0383 0.1980 -0.0044 0.090 Uiso 1 1 calc R U . . . H7B H 0.0586 0.1468 0.0958 0.090 Uiso 1 1 calc R U . . . C8 C 0.1804(11) 0.0799(8) -0.0143(9) 0.069(3) Uani 1 1 d . . . . . C9 C 0.2548(11) 0.0119(8) 0.0448(8) 0.072(3) Uani 1 1 d . . . . . C10 C 0.2780(13) 0.0275(9) 0.1547(9) 0.079(3) Uani 1 1 d . . . . . H10 H 0.2428 0.0854 0.1897 0.095 Uiso 1 1 calc R U . . . C11 C 0.3488(14) -0.0381(9) 0.2096(9) 0.084(3) Uani 1 1 d . . . . . H11 H 0.3619 -0.0260 0.2815 0.101 Uiso 1 1 calc R U . . . C12 C 0.4038(14) -0.1267(10) 0.1567(10) 0.092(3) Uani 1 1 d . . . . . H12 H 0.4538 -0.1723 0.1946 0.110 Uiso 1 1 calc R U . . . C13 C 0.3844(12) -0.1451(9) 0.0529(9) 0.078(3) Uani 1 1 d . . . . . H13 H 0.4215 -0.2038 0.0209 0.093 Uiso 1 1 calc R U . . . C14 C 0.3087(12) -0.0783(8) -0.0112(8) 0.072(3) Uani 1 1 d . . . . . C15 C 0.2821(11) -0.0950(8) -0.1186(8) 0.066(2) Uani 1 1 d . . . . . C16 C 0.2057(12) -0.0273(9) -0.1754(9) 0.075(3) Uani 1 1 d . . . . . C17 C 0.1735(14) -0.0444(11) -0.2860(9) 0.092(3) Uani 1 1 d . . . . . H17 H 0.1976 -0.1057 -0.3224 0.110 Uiso 1 1 calc R U . . . C18 C 0.1096(16) 0.0250(12) -0.3390(11) 0.106(4) Uani 1 1 d . . . . . H18 H 0.0872 0.0107 -0.4111 0.127 Uiso 1 1 calc R U . . . C19 C 0.0760(14) 0.1201(12) -0.2856(11) 0.098(4) Uani 1 1 d . . . . . H19 H 0.0391 0.1702 -0.3230 0.118 Uiso 1 1 calc R U . . . C20 C 0.0963(14) 0.1391(9) -0.1827(10) 0.085(3) Uani 1 1 d . . . . . H20 H 0.0677 0.2006 -0.1495 0.102 Uiso 1 1 calc R U . . . C21 C 0.1614(12) 0.0668(8) -0.1220(9) 0.072(3) Uani 1 1 d . . . . . C22 C 0.3399(13) -0.1881(8) -0.1781(8) 0.080(3) Uani 1 1 d . . . . . H22A H 0.3974 -0.1634 -0.2306 0.096 Uiso 1 1 calc R U . . . H22B H 0.4184 -0.2152 -0.1307 0.096 Uiso 1 1 calc R U . . . C23 C 0.1694(14) -0.3582(9) -0.1832(9) 0.079(3) Uani 1 1 d . . . . . C24 C 0.0356(12) -0.4458(8) -0.2446(8) 0.070(3) Uani 1 1 d . . . . . C25 C -0.0075(14) -0.5342(10) -0.2022(9) 0.086(3) Uani 1 1 d . . . . . H25 H 0.0416 -0.5385 -0.1351 0.103 Uiso 1 1 calc R U . . . C26 C -0.1269(13) -0.6172(9) -0.2625(9) 0.083(3) Uani 1 1 d . . . . . H26 H -0.1581 -0.6786 -0.2364 0.099 Uiso 1 1 calc R U . . . C27 C -0.1970(15) -0.6080(10) -0.3589(9) 0.096(4) Uani 1 1 d . . . . . H27 H -0.2752 -0.6647 -0.3987 0.116 Uiso 1 1 calc R U . . . C28 C -0.0424(13) -0.4406(9) -0.3422(9) 0.078(3) Uani 1 1 d . . . . . H28 H -0.0135 -0.3796 -0.3694 0.094 Uiso 1 1 calc R U . . . C29 C 0.4117(18) 0.1487(11) 0.4913(11) 0.093(3) Uani 1 1 d . . . . . Ag1 Ag 0.69665(11) 0.48910(7) 0.44981(7) 0.0902(4) Uani 1 1 d . . . . . F1 F 0.4580(11) 0.1692(6) 0.5933(6) 0.129(3) Uani 1 1 d . . . . . F2 F 0.5441(10) 0.1409(7) 0.4491(7) 0.137(3) Uani 1 1 d . . . . . F3 F 0.3087(11) 0.0557(6) 0.4626(7) 0.124(3) Uani 1 1 d . . . . . N1 N 0.5811(10) 0.5002(7) 0.2934(7) 0.075(2) Uani 1 1 d . . . . . N2 N -0.1590(11) -0.5200(7) -0.4006(7) 0.082(2) Uani 1 1 d . . . . . O1 O 0.1403(11) 0.3756(6) 0.0056(7) 0.116(3) Uani 1 1 d . . . . . O2 O 0.2509(8) 0.2609(6) 0.0954(6) 0.082(2) Uani 1 1 d . . . . . O3 O 0.1987(8) -0.2761(6) -0.2290(6) 0.0806(19) Uani 1 1 d . . . . . O4 O 0.2485(11) -0.3668(7) -0.1004(6) 0.106(3) Uani 1 1 d . . . . . O5 O 0.2670(12) 0.2256(7) 0.3371(6) 0.112(3) Uani 1 1 d . . . . . O6 O 0.4489(10) 0.3479(6) 0.4821(7) 0.109(3) Uani 1 1 d . . . . . O7 O 0.1803(10) 0.2636(7) 0.5029(7) 0.104(2) Uani 1 1 d . . . . . S1 S 0.3139(4) 0.2569(2) 0.4466(3) 0.0881(9) 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 C1 0.065(6) 0.074(7) 0.069(7) 0.005(5) 0.001(5) 0.022(5) C2 0.064(7) 0.090(9) 0.093(9) -0.010(7) 0.000(6) 0.009(6) C3 0.082(8) 0.074(7) 0.096(9) 0.019(7) 0.007(7) 0.017(6) C4 0.083(7) 0.078(7) 0.075(7) 0.012(6) 0.005(6) 0.026(6) C5 0.061(6) 0.085(7) 0.067(7) 0.001(6) 0.005(5) 0.023(5) C6 0.074(7) 0.078(7) 0.077(8) 0.015(6) 0.005(6) 0.025(6) C7 0.065(6) 0.083(7) 0.073(7) 0.009(6) 0.002(5) 0.016(6) C8 0.045(5) 0.074(6) 0.083(8) 0.006(6) 0.010(5) 0.003(5) C9 0.053(6) 0.081(7) 0.072(7) 0.001(6) -0.010(5) 0.017(5) C10 0.068(6) 0.086(7) 0.073(8) -0.003(6) -0.003(6) 0.017(6) C11 0.085(8) 0.099(8) 0.063(7) 0.004(6) 0.006(6) 0.020(7) C12 0.084(8) 0.094(8) 0.089(9) 0.020(7) -0.011(7) 0.016(7) C13 0.064(6) 0.084(7) 0.076(8) 0.006(6) -0.008(6) 0.016(5) C14 0.053(5) 0.083(7) 0.073(7) 0.011(6) -0.002(5) 0.009(5) C15 0.052(5) 0.067(6) 0.071(7) 0.003(5) 0.001(5) 0.003(5) C16 0.064(6) 0.084(7) 0.074(7) 0.009(6) 0.003(5) 0.017(6) C17 0.083(8) 0.119(10) 0.070(8) 0.016(7) 0.000(6) 0.030(7) C18 0.097(9) 0.130(11) 0.076(9) 0.008(9) -0.006(7) 0.009(8) C19 0.082(8) 0.115(11) 0.086(10) 0.040(9) -0.020(7) -0.003(7) C20 0.081(7) 0.079(7) 0.093(9) 0.018(7) 0.000(7) 0.019(6) C21 0.057(6) 0.081(7) 0.072(7) 0.009(6) 0.005(5) 0.006(5) C22 0.068(6) 0.097(8) 0.063(7) 0.001(6) -0.003(5) 0.010(6) C23 0.082(7) 0.084(8) 0.075(8) 0.018(7) 0.005(6) 0.039(6) C24 0.058(6) 0.067(6) 0.081(7) 0.009(6) -0.003(5) 0.023(5) C25 0.076(7) 0.102(9) 0.075(8) 0.009(7) -0.010(6) 0.032(7) C26 0.078(7) 0.074(7) 0.091(9) 0.016(6) -0.004(7) 0.016(6) C27 0.087(8) 0.103(9) 0.078(8) 0.012(7) -0.024(7) -0.002(7) C28 0.065(6) 0.077(7) 0.084(8) 0.009(6) -0.006(6) 0.011(5) C29 0.097(9) 0.100(10) 0.085(9) 0.008(7) 0.012(8) 0.035(8) Ag1 0.0806(6) 0.0999(7) 0.0771(6) 0.0054(5) -0.0185(4) 0.0215(5) F1 0.158(7) 0.137(6) 0.091(6) 0.030(5) -0.010(5) 0.045(5) F2 0.111(6) 0.146(7) 0.168(8) 0.031(6) 0.035(6) 0.059(5) F3 0.137(6) 0.081(5) 0.145(7) 0.015(5) 0.014(6) 0.007(5) N1 0.065(5) 0.074(6) 0.074(6) 0.004(5) 0.001(5) 0.000(4) N2 0.086(6) 0.075(6) 0.074(6) 0.010(5) -0.012(5) 0.008(5) O1 0.112(6) 0.094(6) 0.120(7) 0.021(5) -0.053(5) 0.021(5) O2 0.071(4) 0.080(5) 0.083(5) -0.001(4) -0.015(4) 0.022(4) O3 0.071(4) 0.081(5) 0.079(5) 0.008(4) -0.007(4) 0.012(4) O4 0.106(6) 0.106(6) 0.083(6) 0.020(5) -0.029(5) -0.001(5) O5 0.140(8) 0.116(6) 0.070(5) 0.003(5) 0.004(5) 0.026(6) O6 0.100(6) 0.083(5) 0.136(8) 0.016(5) 0.002(6) 0.018(5) O7 0.092(6) 0.126(7) 0.095(6) 0.009(5) 0.021(5) 0.034(5) S1 0.091(2) 0.086(2) 0.080(2) 0.0058(16) 0.0004(18) 0.0170(17) _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 C1 N1 1.320(12) . ? C1 C5 1.397(14) . ? C1 H1 0.9300 . ? C2 N1 1.347(13) . ? C2 C3 1.388(16) . ? C2 H2 0.9300 . ? C3 C4 1.381(15) . ? C3 H3 0.9300 . ? C4 C5 1.376(14) . ? C4 H4 0.9300 . ? C5 C6 1.503(14) . ? C6 O1 1.204(12) . ? C6 O2 1.333(11) . ? C7 O2 1.462(11) . ? C7 C8 1.531(13) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C21 1.394(14) . ? C8 C9 1.407(13) . ? C9 C10 1.419(14) . ? C9 C14 1.453(14) . ? C10 C11 1.337(14) . ? C10 H10 0.9300 . ? C11 C12 1.424(15) . ? C11 H11 0.9300 . ? C12 C13 1.341(15) . ? C12 H12 0.9300 . ? C13 C14 1.439(14) . ? C13 H13 0.9300 . ? C14 C15 1.385(14) . ? C15 C16 1.393(14) . ? C15 C22 1.519(14) . ? C16 C17 1.426(15) . ? C16 C21 1.440(14) . ? C17 C18 1.337(16) . ? C17 H17 0.9300 . ? C18 C19 1.412(17) . ? C18 H18 0.9300 . ? C19 C20 1.329(16) . ? C19 H19 0.9300 . ? C20 C21 1.430(14) . ? C20 H20 0.9300 . ? C22 O3 1.493(12) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O4 1.214(12) . ? C23 O3 1.310(12) . ? C23 C24 1.491(15) . ? C24 C28 1.366(14) . ? C24 C25 1.372(14) . ? C25 C26 1.391(15) . ? C25 H25 0.9300 . ? C26 C27 1.347(15) . ? C26 H26 0.9300 . ? C27 N2 1.354(14) . ? C27 H27 0.9300 . ? C28 N2 1.344(13) . ? C28 H28 0.9300 . ? C29 F2 1.318(13) . ? C29 F1 1.320(14) . ? C29 F3 1.328(14) . ? C29 S1 1.842(12) . ? Ag1 N2 2.174(9) 1_666 ? Ag1 N1 2.175(9) . ? N2 Ag1 2.174(9) 1_444 ? O5 S1 1.422(8) . ? O6 S1 1.457(8) . ? O7 S1 1.435(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 N1 C1 C5 121.8(10) . . ? N1 C1 H1 119.1 . . ? C5 C1 H1 119.1 . . ? N1 C2 C3 123.4(11) . . ? N1 C2 H2 118.3 . . ? C3 C2 H2 118.3 . . ? C4 C3 C2 118.0(10) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C5 C4 C3 118.8(10) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C1 119.8(10) . . ? C4 C5 C6 119.5(10) . . ? C1 C5 C6 120.7(10) . . ? O1 C6 O2 124.3(10) . . ? O1 C6 C5 122.7(10) . . ? O2 C6 C5 113.0(9) . . ? O2 C7 C8 112.9(8) . . ? O2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? O2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C21 C8 C9 123.4(10) . . ? C21 C8 C7 119.1(9) . . ? C9 C8 C7 117.5(10) . . ? C8 C9 C10 123.0(10) . . ? C8 C9 C14 117.3(10) . . ? C10 C9 C14 119.6(9) . . ? C11 C10 C9 122.2(10) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? C10 C11 C12 119.3(11) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C13 C12 C11 120.8(11) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 123.0(11) . . ? C12 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C15 C14 C13 125.4(10) . . ? C15 C14 C9 119.5(9) . . ? C13 C14 C9 115.1(10) . . ? C14 C15 C16 122.0(9) . . ? C14 C15 C22 120.1(9) . . ? C16 C15 C22 117.9(10) . . ? C15 C16 C17 122.9(10) . . ? C15 C16 C21 119.8(10) . . ? C17 C16 C21 117.3(10) . . ? C18 C17 C16 122.0(12) . . ? C18 C17 H17 119.0 . . ? C16 C17 H17 119.0 . . ? C17 C18 C19 120.1(13) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 121.1(12) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 121.1(11) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C8 C21 C20 124.1(10) . . ? C8 C21 C16 117.6(9) . . ? C20 C21 C16 118.2(10) . . ? O3 C22 C15 112.3(8) . . ? O3 C22 H22A 109.1 . . ? C15 C22 H22A 109.1 . . ? O3 C22 H22B 109.1 . . ? C15 C22 H22B 109.1 . . ? H22A C22 H22B 107.9 . . ? O4 C23 O3 124.0(11) . . ? O4 C23 C24 121.5(11) . . ? O3 C23 C24 114.4(9) . . ? C28 C24 C25 119.6(10) . . ? C28 C24 C23 121.6(10) . . ? C25 C24 C23 118.8(10) . . ? C24 C25 C26 118.0(10) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? C27 C26 C25 119.5(11) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 N2 123.0(11) . . ? C26 C27 H27 118.5 . . ? N2 C27 H27 118.5 . . ? N2 C28 C24 122.8(10) . . ? N2 C28 H28 118.6 . . ? C24 C28 H28 118.6 . . ? F2 C29 F1 109.0(12) . . ? F2 C29 F3 107.7(11) . . ? F1 C29 F3 109.7(11) . . ? F2 C29 S1 109.1(9) . . ? F1 C29 S1 110.1(9) . . ? F3 C29 S1 111.3(9) . . ? N2 Ag1 N1 172.9(3) 1_666 . ? C1 N1 C2 118.2(9) . . ? C1 N1 Ag1 124.0(7) . . ? C2 N1 Ag1 117.5(7) . . ? C28 N2 C27 117.1(9) . . ? C28 N2 Ag1 124.5(7) . 1_444 ? C27 N2 Ag1 118.3(7) . 1_444 ? C6 O2 C7 118.8(8) . . ? C23 O3 C22 118.6(8) . . ? O5 S1 O7 116.3(6) . . ? O5 S1 O6 115.1(6) . . ? O7 S1 O6 112.2(5) . . ? O5 S1 C29 105.1(6) . . ? O7 S1 C29 104.4(6) . . ? O6 S1 C29 101.7(6) . . ? 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 N1 C2 C3 C4 0.1(17) . . . . ? C2 C3 C4 C5 -1.1(15) . . . . ? C3 C4 C5 C1 1.5(15) . . . . ? C3 C4 C5 C6 -179.1(9) . . . . ? N1 C1 C5 C4 -0.9(15) . . . . ? N1 C1 C5 C6 179.7(9) . . . . ? C4 C5 C6 O1 -21.4(16) . . . . ? C1 C5 C6 O1 158.0(11) . . . . ? C4 C5 C6 O2 160.1(9) . . . . ? C1 C5 C6 O2 -20.5(13) . . . . ? O2 C7 C8 C21 -102.9(10) . . . . ? O2 C7 C8 C9 77.4(11) . . . . ? C21 C8 C9 C10 178.1(9) . . . . ? C7 C8 C9 C10 -2.1(14) . . . . ? C21 C8 C9 C14 -2.1(14) . . . . ? C7 C8 C9 C14 177.6(8) . . . . ? C8 C9 C10 C11 179.9(10) . . . . ? C14 C9 C10 C11 0.1(16) . . . . ? C9 C10 C11 C12 0.3(17) . . . . ? C10 C11 C12 C13 -0.4(18) . . . . ? C11 C12 C13 C14 0.2(18) . . . . ? C12 C13 C14 C15 -178.4(11) . . . . ? C12 C13 C14 C9 0.2(15) . . . . ? C8 C9 C14 C15 -1.4(14) . . . . ? C10 C9 C14 C15 178.4(9) . . . . ? C8 C9 C14 C13 179.8(9) . . . . ? C10 C9 C14 C13 -0.4(13) . . . . ? C13 C14 C15 C16 179.0(10) . . . . ? C9 C14 C15 C16 0.5(15) . . . . ? C13 C14 C15 C22 -2.2(15) . . . . ? C9 C14 C15 C22 179.2(9) . . . . ? C14 C15 C16 C17 -178.5(10) . . . . ? C22 C15 C16 C17 2.7(15) . . . . ? C14 C15 C16 C21 3.9(15) . . . . ? C22 C15 C16 C21 -174.9(9) . . . . ? C15 C16 C17 C18 -175.7(11) . . . . ? C21 C16 C17 C18 2.0(17) . . . . ? C16 C17 C18 C19 2(2) . . . . ? C17 C18 C19 C20 -5(2) . . . . ? C18 C19 C20 C21 3.4(18) . . . . ? C9 C8 C21 C20 -175.6(10) . . . . ? C7 C8 C21 C20 4.7(15) . . . . ? C9 C8 C21 C16 6.3(15) . . . . ? C7 C8 C21 C16 -173.4(8) . . . . ? C19 C20 C21 C8 -177.7(11) . . . . ? C19 C20 C21 C16 0.4(16) . . . . ? C15 C16 C21 C8 -7.1(14) . . . . ? C17 C16 C21 C8 175.1(10) . . . . ? C15 C16 C21 C20 174.7(10) . . . . ? C17 C16 C21 C20 -3.1(14) . . . . ? C14 C15 C22 O3 105.4(10) . . . . ? C16 C15 C22 O3 -75.7(11) . . . . ? O4 C23 C24 C28 -173.5(10) . . . . ? O3 C23 C24 C28 2.9(14) . . . . ? O4 C23 C24 C25 5.3(16) . . . . ? O3 C23 C24 C25 -178.3(9) . . . . ? C28 C24 C25 C26 1.9(15) . . . . ? C23 C24 C25 C26 -177.0(9) . . . . ? C24 C25 C26 C27 -0.7(16) . . . . ? C25 C26 C27 N2 -1.1(19) . . . . ? C25 C24 C28 N2 -1.3(16) . . . . ? C23 C24 C28 N2 177.5(9) . . . . ? C5 C1 N1 C2 -0.1(14) . . . . ? C5 C1 N1 Ag1 173.6(7) . . . . ? C3 C2 N1 C1 0.5(15) . . . . ? C3 C2 N1 Ag1 -173.6(8) . . . . ? C24 C28 N2 C27 -0.5(16) . . . . ? C24 C28 N2 Ag1 174.1(8) . . . 1_444 ? C26 C27 N2 C28 1.7(18) . . . . ? C26 C27 N2 Ag1 -173.2(9) . . . 1_444 ? O1 C6 O2 C7 -4.5(16) . . . . ? C5 C6 O2 C7 173.9(8) . . . . ? C8 C7 O2 C6 122.4(10) . . . . ? O4 C23 O3 C22 1.3(15) . . . . ? C24 C23 O3 C22 -175.0(8) . . . . ? C15 C22 O3 C23 -99.2(10) . . . . ? F2 C29 S1 O5 61.4(11) . . . . ? F1 C29 S1 O5 -179.1(10) . . . . ? F3 C29 S1 O5 -57.3(11) . . . . ? F2 C29 S1 O7 -175.8(9) . . . . ? F1 C29 S1 O7 -56.2(11) . . . . ? F3 C29 S1 O7 65.6(10) . . . . ? F2 C29 S1 O6 -59.0(11) . . . . ? F1 C29 S1 O6 60.6(11) . . . . ? F3 C29 S1 O6 -177.6(9) . . . . ? _refine_diff_density_max 0.671 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.085 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL NV1-complex4 CELL 0.71073 8.2703 12.9164 13.2667 98.584 99.288 98.638 ZERR 2.00 0.0017 0.0027 0.0025 0.016 0.016 0.017 LATT 1 SFAC C H AG F N O S UNIT 58 40 2 6 4 14 2 MERG 2 OMIT 2 1 1 OMIT -2 -10 2 OMIT 0 -12 3 OMIT 2 2 1 OMIT 2 3 2 OMIT -2 2 0 OMIT 2 -11 2 OMIT 5 4 10 OMIT -6 -4 4 OMIT 8 -1 2 OMIT -2 -6 1 FMAP 2 PLAN 5 SIZE 0.020 0.107 0.230 ACTA BOND $H CONF L.S. 10 TEMP 25.00 WGHT 0.055300 2.403300 FVAR 0.36692 C1 1 0.461389 0.426847 0.233850 11.00000 0.06536 0.07373 = 0.06880 0.00516 0.00063 0.02198 AFIX 43 H1 2 0.430508 0.363229 0.256397 11.00000 -1.20000 AFIX 0 C2 1 0.624195 0.591745 0.259333 11.00000 0.06375 0.08984 = 0.09253 -0.00964 0.00012 0.00899 AFIX 43 H2 2 0.709092 0.643227 0.300939 11.00000 -1.20000 AFIX 0 C3 1 0.548473 0.613211 0.165400 11.00000 0.08161 0.07449 = 0.09577 0.01869 0.00675 0.01693 AFIX 43 H3 2 0.581620 0.677350 0.144361 11.00000 -1.20000 AFIX 0 C4 1 0.422416 0.536442 0.104124 11.00000 0.08311 0.07842 = 0.07529 0.01216 0.00500 0.02608 AFIX 43 H4 2 0.367288 0.548228 0.041150 11.00000 -1.20000 AFIX 0 C5 1 0.379868 0.442185 0.137949 11.00000 0.06095 0.08528 = 0.06674 0.00113 0.00480 0.02265 C6 1 0.244640 0.357045 0.071545 11.00000 0.07355 0.07814 = 0.07666 0.01541 0.00498 0.02478 C7 1 0.117131 0.172450 0.044077 11.00000 0.06527 0.08254 = 0.07342 0.00922 0.00249 0.01564 AFIX 23 H7A 2 0.038333 0.198036 -0.004434 11.00000 -1.20000 H7B 2 0.058599 0.146795 0.095753 11.00000 -1.20000 AFIX 0 C8 1 0.180380 0.079924 -0.014335 11.00000 0.04488 0.07352 = 0.08338 0.00620 0.01006 0.00301 C9 1 0.254775 0.011855 0.044776 11.00000 0.05295 0.08142 = 0.07159 0.00069 -0.00967 0.01670 C10 1 0.277976 0.027538 0.154667 11.00000 0.06757 0.08641 = 0.07285 -0.00281 -0.00290 0.01651 AFIX 43 H10 2 0.242763 0.085412 0.189691 11.00000 -1.20000 AFIX 0 C11 1 0.348773 -0.038109 0.209555 11.00000 0.08484 0.09891 = 0.06294 0.00406 0.00581 0.02048 AFIX 43 H11 2 0.361945 -0.026043 0.281533 11.00000 -1.20000 AFIX 0 C12 1 0.403795 -0.126674 0.156691 11.00000 0.08406 0.09411 = 0.08906 0.02038 -0.01108 0.01597 AFIX 43 H12 2 0.453786 -0.172252 0.194606 11.00000 -1.20000 AFIX 0 C13 1 0.384397 -0.145146 0.052902 11.00000 0.06373 0.08390 = 0.07601 0.00555 -0.00791 0.01588 AFIX 43 H13 2 0.421509 -0.203826 0.020888 11.00000 -1.20000 AFIX 0 C14 1 0.308739 -0.078258 -0.011178 11.00000 0.05264 0.08324 = 0.07333 0.01100 -0.00212 0.00896 C15 1 0.282124 -0.094974 -0.118594 11.00000 0.05178 0.06732 = 0.07111 0.00270 0.00117 0.00312 C16 1 0.205660 -0.027283 -0.175387 11.00000 0.06448 0.08370 = 0.07354 0.00873 0.00296 0.01652 C17 1 0.173464 -0.044392 -0.286021 11.00000 0.08322 0.11934 = 0.07042 0.01573 0.00012 0.02979 AFIX 43 H17 2 0.197634 -0.105698 -0.322438 11.00000 -1.20000 AFIX 0 C18 1 0.109597 0.025016 -0.338967 11.00000 0.09692 0.12994 = 0.07643 0.00798 -0.00551 0.00889 AFIX 43 H18 2 0.087244 0.010653 -0.411139 11.00000 -1.20000 AFIX 0 C19 1 0.075992 0.120093 -0.285571 11.00000 0.08181 0.11527 = 0.08643 0.04018 -0.01950 -0.00283 AFIX 43 H19 2 0.039057 0.170178 -0.323016 11.00000 -1.20000 AFIX 0 C20 1 0.096294 0.139148 -0.182693 11.00000 0.08061 0.07862 = 0.09283 0.01829 -0.00006 0.01877 AFIX 43 H20 2 0.067707 0.200588 -0.149533 11.00000 -1.20000 AFIX 0 C21 1 0.161361 0.066798 -0.122048 11.00000 0.05653 0.08068 = 0.07235 0.00903 0.00491 0.00618 C22 1 0.339922 -0.188103 -0.178052 11.00000 0.06814 0.09742 = 0.06304 0.00079 -0.00315 0.01043 AFIX 23 H22A 2 0.397431 -0.163426 -0.230567 11.00000 -1.20000 H22B 2 0.418371 -0.215198 -0.130663 11.00000 -1.20000 AFIX 0 C23 1 0.169392 -0.358236 -0.183233 11.00000 0.08206 0.08409 = 0.07531 0.01782 0.00520 0.03868 C24 1 0.035583 -0.445774 -0.244600 11.00000 0.05847 0.06673 = 0.08096 0.00911 -0.00254 0.02319 C25 1 -0.007544 -0.534185 -0.202167 11.00000 0.07551 0.10151 = 0.07543 0.00912 -0.00971 0.03205 AFIX 43 H25 2 0.041576 -0.538497 -0.135091 11.00000 -1.20000 AFIX 0 C26 1 -0.126909 -0.617166 -0.262455 11.00000 0.07810 0.07391 = 0.09081 0.01597 -0.00434 0.01604 AFIX 43 H26 2 -0.158095 -0.678572 -0.236351 11.00000 -1.20000 AFIX 0 C27 1 -0.197028 -0.607977 -0.358907 11.00000 0.08701 0.10339 = 0.07769 0.01190 -0.02357 -0.00180 AFIX 43 H27 2 -0.275168 -0.664674 -0.398697 11.00000 -1.20000 AFIX 0 C28 1 -0.042370 -0.440612 -0.342217 11.00000 0.06481 0.07652 = 0.08430 0.00852 -0.00597 0.01057 AFIX 43 H28 2 -0.013511 -0.379578 -0.369419 11.00000 -1.20000 AFIX 0 C29 1 0.411717 0.148650 0.491345 11.00000 0.09663 0.09954 = 0.08491 0.00841 0.01196 0.03527 AG1 3 0.696646 0.489100 0.449812 11.00000 0.08062 0.09987 = 0.07712 0.00541 -0.01851 0.02153 F1 4 0.457960 0.169229 0.593284 11.00000 0.15818 0.13682 = 0.09075 0.03005 -0.00997 0.04529 F2 4 0.544078 0.140926 0.449064 11.00000 0.11121 0.14629 = 0.16770 0.03059 0.03547 0.05890 F3 4 0.308662 0.055701 0.462632 11.00000 0.13731 0.08054 = 0.14541 0.01499 0.01426 0.00706 N1 5 0.581057 0.500159 0.293365 11.00000 0.06520 0.07447 = 0.07382 0.00382 0.00120 -0.00044 N2 5 -0.158952 -0.519968 -0.400586 11.00000 0.08559 0.07490 = 0.07394 0.00999 -0.01202 0.00782 O1 6 0.140279 0.375569 0.005569 11.00000 0.11166 0.09373 = 0.11954 0.02128 -0.05325 0.02063 O2 6 0.250921 0.260896 0.095377 11.00000 0.07119 0.08009 = 0.08318 -0.00129 -0.01453 0.02219 O3 6 0.198741 -0.276091 -0.229013 11.00000 0.07128 0.08145 = 0.07942 0.00820 -0.00703 0.01244 O4 6 0.248534 -0.366773 -0.100358 11.00000 0.10610 0.10627 = 0.08329 0.02007 -0.02879 -0.00147 O5 6 0.267029 0.225639 0.337055 11.00000 0.14009 0.11617 = 0.06988 0.00350 0.00435 0.02562 O6 6 0.448949 0.347933 0.482095 11.00000 0.09970 0.08331 = 0.13610 0.01572 0.00246 0.01810 O7 6 0.180333 0.263577 0.502914 11.00000 0.09248 0.12574 = 0.09503 0.00871 0.02053 0.03422 S1 7 0.313857 0.256904 0.446635 11.00000 0.09060 0.08600 = 0.08000 0.00583 0.00040 0.01704 HKLF 4 REM NV1-complex4 REM R1 = 0.0922 for 2560 Fo > 4sig(Fo) and 0.1699 for all 4893 data REM 388 parameters refined using 0 restraints END WGHT 0.0571 2.2665 REM Highest difference peak 0.671, deepest hole -0.715, 1-sigma level 0.085 Q1 1 0.6462 0.4434 0.3638 11.00000 0.05 0.67 Q2 1 0.7262 0.5028 0.3641 11.00000 0.05 0.64 Q3 1 0.6198 0.4234 0.3836 11.00000 0.05 0.64 Q4 1 0.7757 0.5505 0.5141 11.00000 0.05 0.63 Q5 1 0.7287 0.5245 0.5390 11.00000 0.05 0.62 ; _shelx_res_checksum 62621 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_5_CCDC1413540 _database_code_depnum_ccdc_archive 'CCDC 1413540' _audit_update_record ; 2017-07-11 deposited with the CCDC. 2017-07-31 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H20 Ag N2 O4, N O3' _chemical_formula_sum 'C28 H20 Ag N3 O7' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 150(2) _chemical_formula_weight 618.34 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' Ag Ag -0.8971 1.1015 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _chemical_absolute_configuration . loop_ _space_group_symop_operation_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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _cell_length_a 32.985(2) _cell_length_b 5.4535(2) _cell_length_c 14.4690(9) _cell_angle_alpha 90 _cell_angle_beta 112.955(5) _cell_angle_gamma 90 _cell_volume 2396.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22896 _cell_measurement_theta_min 1.53 _cell_measurement_theta_max 29.69 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_F_000 1248 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.180 _exptl_absorpt_coefficient_mu 0.898 _shelx_estimated_absorpt_T_min 0.762 _shelx_estimated_absorpt_T_max 0.855 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8883 _exptl_absorpt_correction_T_max 0.9745 _exptl_absorpt_process_details ; Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany ; _exptl_absorpt_special_details ? _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32569 _diffrn_reflns_av_unetI/netI 0.0243 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.682 _diffrn_reflns_theta_max 29.343 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_point_group_measured_fraction_full 0.989 _reflns_number_total 3213 _reflns_number_gt 2714 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'X-Area (Stoe & Cie, 2009)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2009)' _computing_data_reduction 'X-RED32(Stoe & Cie, 2009)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+17.0462P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_extinction_coef 0.0034(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3213 _refine_ls_number_parameters 194 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.06711(12) 0.8553(7) 0.1469(3) 0.0288(7) Uani 1 1 d . . . . . H1 H 0.0639 0.7443 0.1943 0.035 Uiso 1 1 calc R U . . . C2 C 0.05186(14) 0.9626(8) -0.0173(3) 0.0344(8) Uani 1 1 d . . . . . H2 H 0.0379 0.9259 -0.0868 0.041 Uiso 1 1 calc R U . . . C3 C 0.07637(13) 1.1753(8) 0.0107(3) 0.0332(8) Uani 1 1 d . . . . . H3 H 0.0791 1.2819 -0.0385 0.040 Uiso 1 1 calc R U . . . C4 C 0.09699(12) 1.2302(7) 0.1128(3) 0.0303(7) Uani 1 1 d . . . . . H4 H 0.1135 1.3769 0.1346 0.036 Uiso 1 1 calc R U . . . C5 C 0.09277(11) 1.0645(7) 0.1819(3) 0.0265(7) Uani 1 1 d . . . . . C6 C 0.11426(11) 1.1002(7) 0.2931(3) 0.0270(7) Uani 1 1 d . . . . . C7 C 0.15605(12) 1.3712(7) 0.4236(3) 0.0293(7) Uani 1 1 d . . . . . H7A H 0.1414 1.2787 0.4609 0.035 Uiso 1 1 calc R U . . . H7B H 0.1533 1.5483 0.4351 0.035 Uiso 1 1 calc R U . . . C8 C 0.20394(11) 1.3028(6) 0.4628(2) 0.0264(7) Uani 1 1 d . . . . . C9 C 0.22166(12) 1.1104(6) 0.5324(2) 0.0259(6) Uani 1 1 d . . . . . C10 C 0.19464(13) 0.9584(7) 0.5662(3) 0.0297(7) Uani 1 1 d . . . . . H10 H 0.1639 0.9901 0.5426 0.036 Uiso 1 1 calc R U . . . C11 C 0.21210(13) 0.7694(7) 0.6316(3) 0.0320(8) Uani 1 1 d . . . . . H11 H 0.1934 0.6704 0.6520 0.038 Uiso 1 1 calc R U . . . C12 C 0.25748(14) 0.7197(7) 0.6691(3) 0.0331(8) Uani 1 1 d . . . . . H12 H 0.2693 0.5884 0.7149 0.040 Uiso 1 1 calc R U . . . C13 C 0.28448(13) 0.8599(7) 0.6396(3) 0.0304(7) Uani 1 1 d . . . . . H13 H 0.3151 0.8259 0.6661 0.036 Uiso 1 1 calc R U . . . C14 C 0.26771(12) 1.0586(6) 0.5693(2) 0.0255(6) Uani 1 1 d . . . . . Ag1 Ag 0.0000 0.5000 0.0000 0.0395(2) Uani 1 2 d S . P . . N1 N 0.04671(10) 0.8051(6) 0.0486(2) 0.0312(6) Uani 1 1 d . . . . . O1 O 0.11402(11) 0.9472(6) 0.3521(2) 0.0373(6) Uani 1 1 d . . . . . O2 O 0.13410(8) 1.3176(5) 0.31623(18) 0.0288(5) Uani 1 1 d . . . . . N2 N 0.0000 0.4491(9) 0.2500 0.0332(10) Uani 1 2 d DS T P . . O3 O 0.0201(2) 0.3730(13) 0.1968(5) 0.0400(13) Uani 0.5 1 d . . P A 1 O4 O 0.0177(4) 0.5121(19) 0.3297(7) 0.076(3) Uani 0.5 1 d . . P A 1 O5 O -0.0417(3) 0.441(2) 0.2053(9) 0.077(3) Uani 0.5 1 d D . P A 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 C1 0.0292(16) 0.0264(16) 0.0293(16) -0.0014(13) 0.0097(13) -0.0020(13) C2 0.0322(18) 0.042(2) 0.0281(17) -0.0049(15) 0.0104(14) 0.0009(15) C3 0.0326(17) 0.038(2) 0.0308(17) 0.0014(15) 0.0146(14) -0.0013(15) C4 0.0276(16) 0.0309(17) 0.0326(17) -0.0015(14) 0.0122(14) -0.0028(14) C5 0.0236(15) 0.0261(15) 0.0265(15) -0.0024(13) 0.0061(12) 0.0003(12) C6 0.0257(15) 0.0265(16) 0.0267(15) -0.0026(13) 0.0080(12) -0.0016(13) C7 0.0279(16) 0.0285(17) 0.0258(15) -0.0038(13) 0.0041(13) -0.0008(13) C8 0.0282(16) 0.0240(15) 0.0226(14) -0.0035(12) 0.0052(12) -0.0044(13) C9 0.0295(16) 0.0231(16) 0.0215(14) -0.0032(12) 0.0061(12) -0.0028(13) C10 0.0317(17) 0.0296(17) 0.0253(16) -0.0040(13) 0.0084(13) -0.0064(13) C11 0.0394(19) 0.0316(18) 0.0238(15) -0.0009(13) 0.0112(14) -0.0096(15) C12 0.042(2) 0.0279(17) 0.0249(15) 0.0016(13) 0.0080(14) -0.0035(15) C13 0.0320(17) 0.0244(16) 0.0278(16) -0.0003(13) 0.0040(13) -0.0012(13) C14 0.0311(16) 0.0205(14) 0.0217(14) -0.0031(12) 0.0065(12) -0.0027(12) Ag1 0.0339(3) 0.0352(3) 0.0398(3) -0.00965(17) 0.00400(18) -0.00870(17) N1 0.0292(15) 0.0308(16) 0.0297(14) -0.0060(12) 0.0072(12) -0.0034(12) O1 0.0471(17) 0.0314(14) 0.0270(13) -0.0003(11) 0.0076(12) -0.0087(12) O2 0.0280(12) 0.0255(12) 0.0253(11) -0.0015(9) 0.0024(9) -0.0048(10) N2 0.031(2) 0.033(2) 0.037(2) 0.000 0.0135(19) 0.000 O3 0.036(3) 0.049(4) 0.040(3) -0.014(3) 0.021(2) 0.000(3) O4 0.094(8) 0.093(8) 0.045(5) -0.018(4) 0.032(5) 0.010(5) O5 0.047(4) 0.087(7) 0.098(7) -0.033(6) 0.030(5) -0.008(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 C1 N1 1.344(5) . ? C1 C5 1.393(5) . ? C1 H1 0.9500 . ? C2 N1 1.342(5) . ? C2 C3 1.381(6) . ? C2 H2 0.9500 . ? C3 C4 1.397(5) . ? C3 H3 0.9500 . ? C4 C5 1.394(5) . ? C4 H4 0.9500 . ? C5 C6 1.496(5) . ? C6 O1 1.196(5) . ? C6 O2 1.332(4) . ? C7 O2 1.465(4) . ? C7 C8 1.503(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.413(5) . ? C8 C14 1.415(5) 7_576 ? C9 C14 1.428(5) . ? C9 C10 1.435(5) . ? C10 C11 1.366(5) . ? C10 H10 0.9500 . ? C11 C12 1.405(6) . ? C11 H11 0.9500 . ? C12 C13 1.362(6) . ? C12 H12 0.9500 . ? C13 C14 1.441(5) . ? C13 H13 0.9500 . ? C14 C8 1.415(5) 7_576 ? Ag1 N1 2.189(3) . ? Ag1 N1 2.189(3) 5_565 ? N2 O4 1.125(9) 2 ? N2 O4 1.125(9) . ? N2 O3 1.266(6) . ? N2 O3 1.266(6) 2 ? N2 O5 1.273(9) . ? N2 O5 1.274(9) 2 ? O3 O4 1.381(13) 2 ? O4 O3 1.381(13) 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 N1 C1 C5 122.3(3) . . ? N1 C1 H1 118.9 . . ? C5 C1 H1 118.9 . . ? N1 C2 C3 123.5(4) . . ? N1 C2 H2 118.2 . . ? C3 C2 H2 118.3 . . ? C2 C3 C4 118.5(4) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C1 C5 C4 119.1(3) . . ? C1 C5 C6 117.6(3) . . ? C4 C5 C6 123.3(3) . . ? O1 C6 O2 125.5(3) . . ? O1 C6 C5 123.0(3) . . ? O2 C6 C5 111.5(3) . . ? O2 C7 C8 111.2(3) . . ? O2 C7 H7A 109.4 . . ? C8 C7 H7A 109.4 . . ? O2 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C14 119.2(3) . 7_576 ? C9 C8 C7 122.3(3) . . ? C14 C8 C7 118.4(3) 7_576 . ? C8 C9 C14 119.8(3) . . ? C8 C9 C10 122.2(3) . . ? C14 C9 C10 118.0(3) . . ? C11 C10 C9 121.5(4) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 119.9(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 121.7(4) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C8 C14 C9 120.9(3) 7_576 . ? C8 C14 C13 120.9(3) 7_576 . ? C9 C14 C13 118.2(3) . . ? N1 Ag1 N1 180.0 . 5_565 ? C1 N1 C2 118.1(3) . . ? C1 N1 Ag1 119.6(3) . . ? C2 N1 Ag1 121.8(3) . . ? C6 O2 C7 115.8(3) . . ? O4 N2 O4 144.4(12) 2 . ? O4 N2 O3 70.3(7) 2 . ? O4 N2 O3 122.5(6) . . ? O4 N2 O3 122.5(6) 2 2 ? O4 N2 O3 70.3(7) . 2 ? O3 N2 O3 141.8(8) . 2 ? O5 N2 O5 176.1(12) . 2 ? N2 O3 O4 50.1(4) . 2 ? N2 O4 O3 59.7(6) . 2 ? 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 N1 C2 C3 C4 0.0(6) . . . . ? C2 C3 C4 C5 1.6(6) . . . . ? N1 C1 C5 C4 1.0(6) . . . . ? N1 C1 C5 C6 -179.4(3) . . . . ? C3 C4 C5 C1 -2.1(5) . . . . ? C3 C4 C5 C6 178.4(3) . . . . ? C1 C5 C6 O1 7.7(6) . . . . ? C4 C5 C6 O1 -172.7(4) . . . . ? C1 C5 C6 O2 -173.8(3) . . . . ? C4 C5 C6 O2 5.7(5) . . . . ? O2 C7 C8 C9 -113.1(4) . . . . ? O2 C7 C8 C14 68.7(4) . . . 7_576 ? C14 C8 C9 C14 0.1(5) 7_576 . . . ? C7 C8 C9 C14 -178.0(3) . . . . ? C14 C8 C9 C10 -178.4(3) 7_576 . . . ? C7 C8 C9 C10 3.5(5) . . . . ? C8 C9 C10 C11 178.4(3) . . . . ? C14 C9 C10 C11 -0.1(5) . . . . ? C9 C10 C11 C12 0.9(6) . . . . ? C10 C11 C12 C13 -0.4(6) . . . . ? C11 C12 C13 C14 -0.8(6) . . . . ? C8 C9 C14 C8 -0.1(5) . . . 7_576 ? C10 C9 C14 C8 178.4(3) . . . 7_576 ? C8 C9 C14 C13 -179.6(3) . . . . ? C10 C9 C14 C13 -1.0(5) . . . . ? C12 C13 C14 C8 -177.9(3) . . . 7_576 ? C12 C13 C14 C9 1.5(5) . . . . ? C5 C1 N1 C2 0.6(6) . . . . ? C5 C1 N1 Ag1 -171.7(3) . . . . ? C3 C2 N1 C1 -1.1(6) . . . . ? C3 C2 N1 Ag1 170.9(3) . . . . ? O1 C6 O2 C7 -1.9(5) . . . . ? C5 C6 O2 C7 179.7(3) . . . . ? C8 C7 O2 C6 93.9(4) . . . . ? O4 N2 O3 O4 -142.7(13) . . . 2 ? O3 N2 O3 O4 117.9(6) 2 . . 2 ? O4 N2 O4 O3 118.7(5) 2 . . 2 ? O3 N2 O4 O3 -139.6(9) . . . 2 ? _refine_diff_density_max 3.259 _refine_diff_density_min -0.606 _refine_diff_density_rms 0.145 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL 360 CELL 0.71073 32.9851 5.4535 14.4690 90.000 112.955 90.000 ZERR 4.00 0.0021 0.0002 0.0009 0.000 0.005 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H AG N O UNIT 112 80 4 12 28 MERG 2 OMIT 7 1 1 OMIT -13 3 9 OMIT 0 0 8 OMIT -4 0 10 OMIT 14 2 1 OMIT -26 0 8 OMIT -26 2 9 OMIT -13 3 1 OMIT -8 2 1 OMIT 11 1 1 OMIT -26 0 10 OMIT -5 3 9 OMIT 5 1 1 OMIT -6 4 9 TWIN DELU 0.010 0.010 O3 O4 O5 SIMU 0.040 0.080 1.700 O3 O4 O5 DFIX 1.250 0.020 N2 O5 OMIT -9 3 1 OMIT -13 3 8 OMIT -19 3 1 OMIT 18 2 1 OMIT -12 4 9 OMIT 14 4 1 OMIT -13 3 10 OMIT 22 2 1 OMIT -30 0 10 OMIT -16 0 10 OMIT 31 5 0 FMAP 2 PLAN 5 SIZE 0.180 0.210 0.320 ACTA BOND $H CONF L.S. 50 TEMP -123.10 WGHT 0.089200 17.046202 EXTI 0.003447 BASF 5.93159 FVAR 0.28816 C1 1 0.067113 0.855343 0.146940 11.00000 0.02919 0.02637 = 0.02934 -0.00139 0.00970 -0.00202 AFIX 43 H1 2 0.063924 0.744305 0.194250 11.00000 -1.20000 AFIX 0 C2 1 0.051858 0.962597 -0.017255 11.00000 0.03220 0.04164 = 0.02811 -0.00489 0.01037 0.00090 AFIX 43 H2 2 0.037902 0.925867 -0.086769 11.00000 -1.20000 AFIX 0 C3 1 0.076371 1.175318 0.010655 11.00000 0.03261 0.03814 = 0.03081 0.00140 0.01464 -0.00129 AFIX 43 H3 2 0.079146 1.281908 -0.038482 11.00000 -1.20000 AFIX 0 C4 1 0.096991 1.230161 0.112790 11.00000 0.02765 0.03092 = 0.03259 -0.00152 0.01217 -0.00282 AFIX 43 H4 2 0.113504 1.376878 0.134632 11.00000 -1.20000 AFIX 0 C5 1 0.092769 1.064550 0.181923 11.00000 0.02360 0.02611 = 0.02651 -0.00236 0.00614 0.00030 C6 1 0.114265 1.100195 0.293068 11.00000 0.02574 0.02650 = 0.02675 -0.00256 0.00798 -0.00162 C7 1 0.156049 1.371202 0.423648 11.00000 0.02786 0.02853 = 0.02579 -0.00379 0.00414 -0.00079 AFIX 23 H7A 2 0.141432 1.278742 0.460909 11.00000 -1.20000 H7B 2 0.153253 1.548267 0.435065 11.00000 -1.20000 AFIX 0 C8 1 0.203944 1.302796 0.462814 11.00000 0.02816 0.02400 = 0.02262 -0.00347 0.00521 -0.00439 C9 1 0.221660 1.110368 0.532371 11.00000 0.02949 0.02312 = 0.02146 -0.00325 0.00611 -0.00276 C10 1 0.194641 0.958449 0.566204 11.00000 0.03171 0.02957 = 0.02527 -0.00403 0.00840 -0.00636 AFIX 43 H10 2 0.163934 0.990110 0.542575 11.00000 -1.20000 AFIX 0 C11 1 0.212104 0.769428 0.631604 11.00000 0.03945 0.03165 = 0.02381 -0.00087 0.01118 -0.00962 AFIX 43 H11 2 0.193370 0.670448 0.651999 11.00000 -1.20000 AFIX 0 C12 1 0.257484 0.719706 0.669076 11.00000 0.04199 0.02788 = 0.02487 0.00162 0.00799 -0.00354 AFIX 43 H12 2 0.269318 0.588418 0.714885 11.00000 -1.20000 AFIX 0 C13 1 0.284477 0.859940 0.639644 11.00000 0.03198 0.02439 = 0.02776 -0.00027 0.00397 -0.00117 AFIX 43 H13 2 0.315149 0.825874 0.666143 11.00000 -1.20000 AFIX 0 C14 1 0.267709 1.058647 0.569345 11.00000 0.03106 0.02046 = 0.02166 -0.00309 0.00650 -0.00271 AG1 3 0.000000 0.500000 0.000000 10.50000 0.03395 0.03518 = 0.03981 -0.00965 0.00400 -0.00870 N1 4 0.046707 0.805085 0.048567 11.00000 0.02921 0.03080 = 0.02969 -0.00596 0.00724 -0.00344 O1 5 0.114016 0.947246 0.352113 11.00000 0.04712 0.03142 = 0.02703 -0.00029 0.00764 -0.00874 O2 5 0.134099 1.317602 0.316230 11.00000 0.02804 0.02553 = 0.02530 -0.00149 0.00237 -0.00477 N2 4 0.000000 0.449060 0.250000 10.50000 0.03071 0.03274 = 0.03651 0.00000 0.01354 0.00000 PART 1 O3 5 0.020134 0.373042 0.196823 10.50000 0.03632 0.04855 = 0.04038 -0.01403 0.02076 -0.00045 O4 5 0.017701 0.512094 0.329742 10.50000 0.09369 0.09303 = 0.04509 -0.01831 0.03230 0.00970 PART 2 O5 5 -0.041748 0.441104 0.205316 10.50000 0.04730 0.08688 = 0.09838 -0.03276 0.02969 -0.00757 HKLF 4 REM 360 REM R1 = 0.0529 for 2714 Fo > 4sig(Fo) and 0.0622 for all 3213 data REM 194 parameters refined using 1 restraints END WGHT 0.0819 14.0599 REM Highest difference peak 3.259, deepest hole -0.606, 1-sigma level 0.145 Q1 1 0.0000 0.4985 0.3896 11.00000 0.05 3.26 Q2 1 0.0000 0.7074 0.2500 10.50000 0.05 0.74 Q3 1 0.2110 0.6657 0.5194 11.00000 0.05 0.54 Q4 1 -0.0283 0.5411 0.0271 11.00000 0.05 0.48 Q5 1 0.2851 0.8429 0.5824 11.00000 0.05 0.45 ; _shelx_res_checksum 2787 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_complex1 _database_code_depnum_ccdc_archive 'CCDC 1413538' _audit_update_record ; 2015-07-17 deposited with the CCDC. 2017-07-31 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 Ag N3 O7, C H4 O' _chemical_formula_sum 'C29 H24 Ag N3 O8' _chemical_formula_weight 650.38 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' Ag Ag -0.8971 1.1015 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2044(4) _cell_length_b 9.4246(4) _cell_length_c 16.7815(8) _cell_angle_alpha 93.942(4) _cell_angle_beta 96.876(4) _cell_angle_gamma 91.701(4) _cell_volume 1284.28(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23307 _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 25.07 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_F_000 660 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_absorpt_coefficient_mu 0.845 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21429 _diffrn_reflns_av_unetI/netI 0.0683 _diffrn_reflns_av_R_equivalents 0.1374 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.225 _diffrn_reflns_theta_max 24.579 _diffrn_reflns_theta_full 24.579 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 4296 _reflns_number_gt 3622 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'X-Area (Stoe & Cie, 2009)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2009)' _computing_data_reduction 'X-RED32(Stoe & Cie, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+1.1304P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4296 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.27567(5) 0.50748(4) 0.97665(2) 0.03838(19) Uani 1 1 d . . . . . O1 O 0.3487(6) 0.9004(4) 0.6612(3) 0.0524(11) Uani 1 1 d . . . . . O2 O 0.4117(4) 0.6741(4) 0.6813(2) 0.0313(8) Uani 1 1 d . . . . . O3 O 0.0882(4) 0.3762(4) 0.2643(2) 0.0311(8) Uani 1 1 d . . . . . O4 O 0.1695(5) 0.1625(4) 0.3016(2) 0.0449(10) Uani 1 1 d . . . . . O5 O 0.1396(5) 0.2784(5) 0.8589(3) 0.0537(11) Uani 1 1 d . . . . . O6 O -0.0959(5) 0.1818(4) 0.8729(3) 0.0444(9) Uani 1 1 d . . . . . O7 O -0.0280(5) 0.3943(4) 0.9268(3) 0.0465(10) Uani 1 1 d . . . . . N1 N 0.2545(5) 0.6865(5) 0.9018(3) 0.0323(9) Uani 1 1 d . . . . . N2 N 0.3027(5) 0.3357(4) 0.0572(3) 0.0332(9) Uani 1 1 d . . . . . N3 N 0.0053(6) 0.2844(5) 0.8846(3) 0.0375(10) Uani 1 1 d . . . . . C1 C 0.1814(6) 0.8036(6) 0.9289(3) 0.0345(11) Uani 1 1 d . . . . . H1 H 0.1428 0.8043 0.9789 0.041 Uiso 1 1 calc R U . . . C2 C 0.1614(7) 0.9226(6) 0.8854(3) 0.0373(12) Uani 1 1 d . . . . . H2 H 0.1109 1.0017 0.9060 0.045 Uiso 1 1 calc R U . . . C3 C 0.2173(7) 0.9228(5) 0.8106(3) 0.0340(11) Uani 1 1 d . . . . . H3 H 0.2054 1.0016 0.7803 0.041 Uiso 1 1 calc R U . . . C4 C 0.2917(6) 0.8021(5) 0.7823(3) 0.0291(10) Uani 1 1 d . . . . . C5 C 0.3087(6) 0.6868(5) 0.8295(3) 0.0307(11) Uani 1 1 d . . . . . H5 H 0.3594 0.6068 0.8102 0.037 Uiso 1 1 calc R U . . . C6 C 0.3538(6) 0.8006(5) 0.7019(3) 0.0314(11) Uani 1 1 d . . . . . C7 C 0.4700(6) 0.6561(5) 0.6017(3) 0.0315(11) Uani 1 1 d . . . . . H7A H 0.5618 0.5935 0.6047 0.038 Uiso 1 1 calc R U . . . H7B H 0.5089 0.7478 0.5869 0.038 Uiso 1 1 calc R U . . . C8 C 0.3376(6) 0.5952(5) 0.5373(3) 0.0270(10) Uani 1 1 d . . . . . C9 C 0.2791(6) 0.4550(5) 0.5405(3) 0.0286(10) Uani 1 1 d . . . . . C10 C 0.3321(6) 0.3721(5) 0.6067(3) 0.0309(11) Uani 1 1 d . . . . . H10 H 0.4063 0.4130 0.6489 0.037 Uiso 1 1 calc R U . . . C11 C 0.2766(7) 0.2358(5) 0.6094(3) 0.0353(12) Uani 1 1 d . . . . . H11 H 0.3125 0.1848 0.6533 0.042 Uiso 1 1 calc R U . . . C12 C 0.1653(7) 0.1709(5) 0.5464(3) 0.0357(12) Uani 1 1 d . . . . . H12 H 0.1282 0.0774 0.5492 0.043 Uiso 1 1 calc R U . . . C13 C 0.1112(6) 0.2418(5) 0.4818(3) 0.0321(11) Uani 1 1 d . . . . . H13 H 0.0373 0.1968 0.4408 0.038 Uiso 1 1 calc R U . . . C14 C 0.1672(6) 0.3872(5) 0.4757(3) 0.0271(10) Uani 1 1 d . . . . . C15 C 0.1189(6) 0.4632(5) 0.4076(3) 0.0275(10) Uani 1 1 d . . . . . C16 C 0.1749(6) 0.6062(5) 0.4043(3) 0.0277(10) Uani 1 1 d . . . . . C17 C 0.1270(6) 0.6864(5) 0.3366(3) 0.0322(11) Uani 1 1 d . . . . . H17 H 0.0604 0.6430 0.2924 0.039 Uiso 1 1 calc R U . . . C18 C 0.1770(7) 0.8244(6) 0.3356(3) 0.0372(12) Uani 1 1 d . . . . . H18 H 0.1429 0.8750 0.2913 0.045 Uiso 1 1 calc R U . . . C19 C 0.2805(7) 0.8921(5) 0.4015(3) 0.0382(12) Uani 1 1 d . . . . . H19 H 0.3133 0.9871 0.4000 0.046 Uiso 1 1 calc R U . . . C20 C 0.3331(7) 0.8208(5) 0.4670(3) 0.0357(12) Uani 1 1 d . . . . . H20 H 0.4016 0.8671 0.5096 0.043 Uiso 1 1 calc R U . . . C21 C 0.2829(6) 0.6738(5) 0.4704(3) 0.0283(10) Uani 1 1 d . . . . . C22 C 0.0055(6) 0.3967(5) 0.3371(3) 0.0300(10) Uani 1 1 d . . . . . H22A H -0.0366 0.3053 0.3507 0.036 Uiso 1 1 calc R U . . . H22B H -0.0871 0.4570 0.3262 0.036 Uiso 1 1 calc R U . . . C23 C 0.1632(6) 0.2533(5) 0.2551(3) 0.0306(11) Uani 1 1 d . . . . . C24 C 0.2361(6) 0.2397(5) 0.1775(3) 0.0291(10) Uani 1 1 d . . . . . C25 C 0.2981(6) 0.1085(5) 0.1540(3) 0.0321(11) Uani 1 1 d . . . . . H25 H 0.2970 0.0329 0.1868 0.039 Uiso 1 1 calc R U . . . C26 C 0.3610(6) 0.0936(5) 0.0810(3) 0.0342(11) Uani 1 1 d . . . . . H26 H 0.4022 0.0075 0.0637 0.041 Uiso 1 1 calc R U . . . C27 C 0.3616(6) 0.2086(5) 0.0346(3) 0.0325(11) Uani 1 1 d . . . . . H27 H 0.4043 0.1984 -0.0143 0.039 Uiso 1 1 calc R U . . . C28 C 0.2404(6) 0.3493(5) 0.1271(3) 0.0312(11) Uani 1 1 d . . . . . H28 H 0.1982 0.4360 0.1425 0.037 Uiso 1 1 calc R U . . . O8 O 0.4118(5) 0.7317(5) 0.1100(3) 0.0527(11) Uani 1 1 d . . . . . H8 H 0.3075 0.7470 0.1157 0.079 Uiso 1 1 d R U . . . C29 C 0.4808(8) 0.7097(8) 0.1894(4) 0.0525(16) Uani 1 1 d . . . . . H29A H 0.5926 0.6824 0.1891 0.079 Uiso 1 1 calc R U . . . H29B H 0.4187 0.6357 0.2100 0.079 Uiso 1 1 calc R U . . . H29C H 0.4781 0.7961 0.2229 0.079 Uiso 1 1 calc R U . . . 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 0.0486(3) 0.0300(3) 0.0389(3) 0.01186(16) 0.00990(18) 0.00135(17) O1 0.086(3) 0.032(2) 0.048(2) 0.0158(18) 0.028(2) 0.017(2) O2 0.0369(19) 0.0258(18) 0.0327(19) 0.0045(14) 0.0088(15) 0.0043(14) O3 0.0356(19) 0.0258(17) 0.0331(18) 0.0045(14) 0.0064(15) 0.0056(14) O4 0.071(3) 0.032(2) 0.038(2) 0.0168(17) 0.0215(19) 0.0156(18) O5 0.043(2) 0.056(3) 0.064(3) -0.005(2) 0.023(2) 0.0034(19) O6 0.042(2) 0.033(2) 0.056(2) -0.0027(17) 0.0022(19) -0.0019(17) O7 0.042(2) 0.034(2) 0.064(3) -0.0037(18) 0.0109(19) 0.0063(16) N1 0.032(2) 0.033(2) 0.032(2) 0.0065(17) 0.0038(18) -0.0001(17) N2 0.037(2) 0.027(2) 0.036(2) 0.0049(17) 0.0065(19) 0.0008(17) N3 0.037(3) 0.034(3) 0.041(3) 0.0060(19) 0.003(2) 0.0076(19) C1 0.036(3) 0.039(3) 0.030(3) 0.003(2) 0.008(2) 0.004(2) C2 0.037(3) 0.033(3) 0.043(3) 0.002(2) 0.006(2) 0.011(2) C3 0.040(3) 0.025(3) 0.037(3) 0.009(2) 0.002(2) 0.002(2) C4 0.033(3) 0.023(2) 0.031(3) 0.0038(19) 0.002(2) -0.0017(19) C5 0.032(3) 0.024(2) 0.036(3) 0.005(2) 0.001(2) 0.0043(19) C6 0.032(3) 0.025(3) 0.037(3) 0.002(2) 0.003(2) 0.0023(19) C7 0.029(3) 0.029(3) 0.038(3) 0.004(2) 0.010(2) 0.0034(19) C8 0.027(2) 0.026(2) 0.029(2) 0.0023(19) 0.007(2) 0.0047(18) C9 0.024(2) 0.026(2) 0.037(3) 0.004(2) 0.010(2) 0.0044(18) C10 0.035(3) 0.030(3) 0.029(3) 0.003(2) 0.004(2) 0.006(2) C11 0.040(3) 0.028(3) 0.039(3) 0.009(2) 0.008(2) 0.007(2) C12 0.044(3) 0.022(2) 0.044(3) 0.007(2) 0.014(2) 0.000(2) C13 0.037(3) 0.027(3) 0.034(3) 0.003(2) 0.011(2) 0.004(2) C14 0.025(2) 0.024(2) 0.034(3) 0.0003(19) 0.010(2) 0.0035(18) C15 0.027(2) 0.027(2) 0.030(2) 0.0034(19) 0.009(2) 0.0049(19) C16 0.026(2) 0.024(2) 0.034(3) 0.0048(19) 0.007(2) 0.0046(18) C17 0.034(3) 0.034(3) 0.030(3) 0.004(2) 0.008(2) 0.009(2) C18 0.046(3) 0.031(3) 0.037(3) 0.010(2) 0.009(2) 0.007(2) C19 0.049(3) 0.021(2) 0.047(3) 0.005(2) 0.015(3) 0.002(2) C20 0.041(3) 0.028(3) 0.040(3) 0.007(2) 0.011(2) 0.001(2) C21 0.027(2) 0.024(2) 0.035(3) 0.0033(19) 0.010(2) 0.0031(18) C22 0.027(2) 0.034(3) 0.030(3) 0.003(2) 0.008(2) 0.0048(19) C23 0.029(3) 0.027(3) 0.035(3) -0.001(2) 0.004(2) 0.0041(19) C24 0.027(2) 0.025(2) 0.036(3) 0.006(2) 0.003(2) 0.0021(18) C25 0.034(3) 0.023(2) 0.041(3) 0.005(2) 0.004(2) 0.0042(19) C26 0.034(3) 0.026(3) 0.042(3) -0.003(2) 0.006(2) 0.007(2) C27 0.032(3) 0.031(3) 0.035(3) 0.000(2) 0.007(2) 0.004(2) C28 0.035(3) 0.026(2) 0.035(3) 0.005(2) 0.007(2) 0.0031(19) O8 0.042(2) 0.076(3) 0.042(2) 0.012(2) 0.0108(19) 0.006(2) C29 0.038(3) 0.072(5) 0.048(4) 0.010(3) 0.005(3) 0.008(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 2.170(4) . ? Ag1 N2 2.179(4) 1_556 ? O1 C6 1.198(7) . ? O2 C6 1.336(6) . ? O2 C7 1.472(6) . ? O3 C23 1.336(6) . ? O3 C22 1.472(6) . ? O4 C23 1.195(7) . ? O5 N3 1.231(6) . ? O6 N3 1.245(6) . ? O7 N3 1.269(6) . ? N1 C5 1.343(7) . ? N1 C1 1.349(7) . ? N2 C28 1.334(7) . ? N2 C27 1.352(7) . ? N2 Ag1 2.179(4) 1_554 ? C1 C2 1.383(8) . ? C1 H1 0.9300 . ? C2 C3 1.386(8) . ? C2 H2 0.9300 . ? C3 C4 1.389(7) . ? C3 H3 0.9300 . ? C4 C5 1.388(7) . ? C4 C6 1.497(7) . ? C5 H5 0.9300 . ? C7 C8 1.507(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.400(7) . ? C8 C21 1.423(7) . ? C9 C10 1.434(7) . ? C9 C14 1.438(7) . ? C10 C11 1.356(7) . ? C10 H10 0.9300 . ? C11 C12 1.405(8) . ? C11 H11 0.9300 . ? C12 C13 1.349(7) . ? C12 H12 0.9300 . ? C13 C14 1.446(7) . ? C13 H13 0.9300 . ? C14 C15 1.412(7) . ? C15 C16 1.418(7) . ? C15 C22 1.503(7) . ? C16 C17 1.430(7) . ? C16 C21 1.434(7) . ? C17 C18 1.353(8) . ? C17 H17 0.9300 . ? C18 C19 1.413(8) . ? C18 H18 0.9300 . ? C19 C20 1.360(8) . ? C19 H19 0.9300 . ? C20 C21 1.441(7) . ? C20 H20 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.496(7) . ? C24 C28 1.382(7) . ? C24 C25 1.400(7) . ? C25 C26 1.385(8) . ? C25 H25 0.9300 . ? C26 C27 1.378(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? O8 C29 1.416(7) . ? O8 H8 0.8876 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 176.90(15) . 1_556 ? C6 O2 C7 117.0(4) . . ? C23 O3 C22 116.0(4) . . ? C5 N1 C1 117.9(4) . . ? C5 N1 Ag1 123.6(3) . . ? C1 N1 Ag1 118.4(3) . . ? C28 N2 C27 118.4(4) . . ? C28 N2 Ag1 119.0(3) . 1_554 ? C27 N2 Ag1 122.1(4) . 1_554 ? O5 N3 O6 121.1(5) . . ? O5 N3 O7 119.6(5) . . ? O6 N3 O7 119.2(5) . . ? N1 C1 C2 122.6(5) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 119.4(5) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 118.2(5) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C3 C4 C5 119.3(5) . . ? C3 C4 C6 119.0(4) . . ? C5 C4 C6 121.7(4) . . ? N1 C5 C4 122.5(5) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? O1 C6 O2 124.9(5) . . ? O1 C6 C4 123.7(5) . . ? O2 C6 C4 111.4(4) . . ? O2 C7 C8 112.4(4) . . ? O2 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? O2 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C21 120.0(5) . . ? C9 C8 C7 118.9(4) . . ? C21 C8 C7 120.8(4) . . ? C8 C9 C10 121.7(5) . . ? C8 C9 C14 120.7(5) . . ? C10 C9 C14 117.6(4) . . ? C11 C10 C9 121.7(5) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 120.5(5) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 121.2(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C9 119.1(4) . . ? C15 C14 C13 122.4(5) . . ? C9 C14 C13 118.5(4) . . ? C14 C15 C16 120.7(4) . . ? C14 C15 C22 121.5(4) . . ? C16 C15 C22 117.8(4) . . ? C15 C16 C17 122.0(5) . . ? C15 C16 C21 119.6(4) . . ? C17 C16 C21 118.4(5) . . ? C18 C17 C16 121.2(5) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 121.2(5) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 120.2(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C8 C21 C16 119.7(4) . . ? C8 C21 C20 121.7(5) . . ? C16 C21 C20 118.5(5) . . ? O3 C22 C15 112.2(4) . . ? O3 C22 H22A 109.2 . . ? C15 C22 H22A 109.2 . . ? O3 C22 H22B 109.2 . . ? C15 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O4 C23 O3 125.0(5) . . ? O4 C23 C24 123.2(5) . . ? O3 C23 C24 111.8(4) . . ? C28 C24 C25 118.8(5) . . ? C28 C24 C23 122.9(4) . . ? C25 C24 C23 118.3(4) . . ? C26 C25 C24 118.7(5) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C27 C26 C25 118.9(4) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? N2 C27 C26 122.6(5) . . ? N2 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? N2 C28 C24 122.7(5) . . ? N2 C28 H28 118.7 . . ? C24 C28 H28 118.7 . . ? C29 O8 H8 102.6 . . ? O8 C29 H29A 109.5 . . ? O8 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O8 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 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 C1 C2 -0.3(8) . . . . ? Ag1 N1 C1 C2 -179.6(4) . . . . ? N1 C1 C2 C3 0.4(8) . . . . ? C1 C2 C3 C4 0.1(8) . . . . ? C2 C3 C4 C5 -0.5(8) . . . . ? C2 C3 C4 C6 -179.7(5) . . . . ? C1 N1 C5 C4 -0.1(7) . . . . ? Ag1 N1 C5 C4 179.2(4) . . . . ? C3 C4 C5 N1 0.5(8) . . . . ? C6 C4 C5 N1 179.7(4) . . . . ? C7 O2 C6 O1 -1.4(8) . . . . ? C7 O2 C6 C4 177.4(4) . . . . ? C3 C4 C6 O1 3.0(8) . . . . ? C5 C4 C6 O1 -176.2(5) . . . . ? C3 C4 C6 O2 -175.9(4) . . . . ? C5 C4 C6 O2 5.0(7) . . . . ? C6 O2 C7 C8 -92.7(5) . . . . ? O2 C7 C8 C9 -67.4(6) . . . . ? O2 C7 C8 C21 118.2(5) . . . . ? C21 C8 C9 C10 179.6(4) . . . . ? C7 C8 C9 C10 5.1(7) . . . . ? C21 C8 C9 C14 1.8(7) . . . . ? C7 C8 C9 C14 -172.7(4) . . . . ? C8 C9 C10 C11 -179.3(5) . . . . ? C14 C9 C10 C11 -1.4(7) . . . . ? C9 C10 C11 C12 0.5(8) . . . . ? C10 C11 C12 C13 0.2(8) . . . . ? C11 C12 C13 C14 0.2(8) . . . . ? C8 C9 C14 C15 1.1(7) . . . . ? C10 C9 C14 C15 -176.8(4) . . . . ? C8 C9 C14 C13 179.6(4) . . . . ? C10 C9 C14 C13 1.7(6) . . . . ? C12 C13 C14 C15 177.3(5) . . . . ? C12 C13 C14 C9 -1.1(7) . . . . ? C9 C14 C15 C16 -2.3(7) . . . . ? C13 C14 C15 C16 179.3(4) . . . . ? C9 C14 C15 C22 178.5(4) . . . . ? C13 C14 C15 C22 0.0(7) . . . . ? C14 C15 C16 C17 -179.4(4) . . . . ? C22 C15 C16 C17 -0.1(7) . . . . ? C14 C15 C16 C21 0.6(7) . . . . ? C22 C15 C16 C21 179.9(4) . . . . ? C15 C16 C17 C18 177.6(5) . . . . ? C21 C16 C17 C18 -2.4(7) . . . . ? C16 C17 C18 C19 1.1(8) . . . . ? C17 C18 C19 C20 0.3(8) . . . . ? C18 C19 C20 C21 -0.3(8) . . . . ? C9 C8 C21 C16 -3.5(7) . . . . ? C7 C8 C21 C16 170.9(4) . . . . ? C9 C8 C21 C20 176.5(4) . . . . ? C7 C8 C21 C20 -9.1(7) . . . . ? C15 C16 C21 C8 2.3(7) . . . . ? C17 C16 C21 C8 -177.7(4) . . . . ? C15 C16 C21 C20 -177.7(4) . . . . ? C17 C16 C21 C20 2.3(7) . . . . ? C19 C20 C21 C8 179.0(5) . . . . ? C19 C20 C21 C16 -1.1(7) . . . . ? C23 O3 C22 C15 88.4(5) . . . . ? C14 C15 C22 O3 -113.0(5) . . . . ? C16 C15 C22 O3 67.7(5) . . . . ? C22 O3 C23 O4 -1.2(7) . . . . ? C22 O3 C23 C24 177.2(4) . . . . ? O4 C23 C24 C28 -174.5(5) . . . . ? O3 C23 C24 C28 7.0(7) . . . . ? O4 C23 C24 C25 7.4(8) . . . . ? O3 C23 C24 C25 -171.0(4) . . . . ? C28 C24 C25 C26 -0.2(7) . . . . ? C23 C24 C25 C26 178.0(4) . . . . ? C24 C25 C26 C27 0.6(7) . . . . ? C28 N2 C27 C26 -0.5(8) . . . . ? Ag1 N2 C27 C26 -172.0(4) 1_554 . . . ? C25 C26 C27 N2 -0.2(8) . . . . ? C27 N2 C28 C24 1.0(7) . . . . ? Ag1 N2 C28 C24 172.7(4) 1_554 . . . ? C25 C24 C28 N2 -0.6(8) . . . . ? C23 C24 C28 N2 -178.7(5) . . . . ? _refine_diff_density_max 1.541 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.153 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL 1 in P1 New: New: P-1 CELL 0.71073 8.2044 9.4246 16.7815 93.942 96.876 91.701 ZERR 2.00 0.0004 0.0004 0.0008 0.004 0.004 0.004 LATT 1 SFAC C H AG N O UNIT 58 48 2 6 16 MERG 2 OMIT 0.00 50.00 OMIT 2 -6 9 OMIT -1 9 0 OMIT 3 -4 7 FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 5 WGHT 0.090200 1.130400 FVAR 0.42815 AG1 3 0.275666 0.507477 0.976650 11.00000 0.04860 0.03000 = 0.03893 0.01186 0.00990 0.00135 O1 5 0.348740 0.900405 0.661214 11.00000 0.08561 0.03150 = 0.04777 0.01577 0.02806 0.01700 O2 5 0.411689 0.674128 0.681265 11.00000 0.03694 0.02575 = 0.03275 0.00445 0.00877 0.00425 O3 5 0.088191 0.376164 0.264278 11.00000 0.03561 0.02585 = 0.03308 0.00454 0.00640 0.00555 O4 5 0.169474 0.162532 0.301594 11.00000 0.07052 0.03246 = 0.03815 0.01680 0.02146 0.01563 O5 5 0.139621 0.278378 0.858944 11.00000 0.04301 0.05648 = 0.06447 -0.00455 0.02341 0.00335 O6 5 -0.095911 0.181770 0.872901 11.00000 0.04162 0.03327 = 0.05645 -0.00267 0.00222 -0.00195 O7 5 -0.027959 0.394281 0.926799 11.00000 0.04237 0.03369 = 0.06393 -0.00370 0.01087 0.00627 N1 4 0.254499 0.686460 0.901845 11.00000 0.03197 0.03313 = 0.03233 0.00647 0.00380 -0.00007 N2 4 0.302653 0.335659 0.057202 11.00000 0.03669 0.02749 = 0.03637 0.00491 0.00646 0.00083 N3 4 0.005319 0.284393 0.884590 11.00000 0.03743 0.03419 = 0.04125 0.00598 0.00340 0.00762 C1 1 0.181370 0.803592 0.928919 11.00000 0.03558 0.03883 = 0.03019 0.00283 0.00754 0.00381 AFIX 43 H1 2 0.142841 0.804343 0.978852 11.00000 -1.20000 AFIX 0 C2 1 0.161403 0.922616 0.885378 11.00000 0.03749 0.03265 = 0.04262 0.00207 0.00649 0.01082 AFIX 43 H2 2 0.110945 1.001739 0.906047 11.00000 -1.20000 AFIX 0 C3 1 0.217350 0.922791 0.810633 11.00000 0.04012 0.02538 = 0.03661 0.00889 0.00160 0.00195 AFIX 43 H3 2 0.205373 1.001596 0.780290 11.00000 -1.20000 AFIX 0 C4 1 0.291747 0.802135 0.782296 11.00000 0.03255 0.02296 = 0.03145 0.00377 0.00236 -0.00166 C5 1 0.308661 0.686824 0.829457 11.00000 0.03178 0.02445 = 0.03572 0.00472 0.00136 0.00432 AFIX 43 H5 2 0.359446 0.606774 0.810173 11.00000 -1.20000 AFIX 0 C6 1 0.353754 0.800649 0.701893 11.00000 0.03170 0.02538 = 0.03699 0.00181 0.00346 0.00230 C7 1 0.469971 0.656147 0.601674 11.00000 0.02869 0.02912 = 0.03847 0.00373 0.01004 0.00343 AFIX 23 H7A 2 0.561850 0.593490 0.604745 11.00000 -1.20000 H7B 2 0.508892 0.747777 0.586929 11.00000 -1.20000 AFIX 0 C8 1 0.337617 0.595207 0.537340 11.00000 0.02695 0.02601 = 0.02915 0.00230 0.00724 0.00466 C9 1 0.279085 0.454960 0.540546 11.00000 0.02438 0.02648 = 0.03685 0.00364 0.00976 0.00435 C10 1 0.332083 0.372134 0.606745 11.00000 0.03466 0.02968 = 0.02880 0.00323 0.00376 0.00640 AFIX 43 H10 2 0.406343 0.412965 0.648886 11.00000 -1.20000 AFIX 0 C11 1 0.276647 0.235776 0.609447 11.00000 0.04049 0.02810 = 0.03923 0.00912 0.00757 0.00728 AFIX 43 H11 2 0.312547 0.184842 0.653344 11.00000 -1.20000 AFIX 0 C12 1 0.165310 0.170886 0.546368 11.00000 0.04384 0.02189 = 0.04414 0.00674 0.01402 0.00020 AFIX 43 H12 2 0.128249 0.077361 0.549188 11.00000 -1.20000 AFIX 0 C13 1 0.111226 0.241834 0.481792 11.00000 0.03661 0.02738 = 0.03420 0.00336 0.01103 0.00418 AFIX 43 H13 2 0.037291 0.196843 0.440840 11.00000 -1.20000 AFIX 0 C14 1 0.167152 0.387158 0.475676 11.00000 0.02478 0.02391 = 0.03395 0.00026 0.01004 0.00349 C15 1 0.118851 0.463204 0.407648 11.00000 0.02702 0.02740 = 0.02983 0.00343 0.00873 0.00491 C16 1 0.174887 0.606232 0.404302 11.00000 0.02647 0.02419 = 0.03402 0.00484 0.00733 0.00461 C17 1 0.127036 0.686439 0.336597 11.00000 0.03446 0.03370 = 0.03019 0.00447 0.00753 0.00907 AFIX 43 H17 2 0.060360 0.642969 0.292403 11.00000 -1.20000 AFIX 0 C18 1 0.176957 0.824410 0.335629 11.00000 0.04563 0.03095 = 0.03724 0.01002 0.00890 0.00718 AFIX 43 H18 2 0.142873 0.874988 0.291331 11.00000 -1.20000 AFIX 0 C19 1 0.280511 0.892092 0.401476 11.00000 0.04927 0.02109 = 0.04691 0.00451 0.01493 0.00199 AFIX 43 H19 2 0.313316 0.987090 0.400024 11.00000 -1.20000 AFIX 0 C20 1 0.333089 0.820828 0.466950 11.00000 0.04127 0.02803 = 0.03997 0.00666 0.01131 0.00094 AFIX 43 H20 2 0.401629 0.867124 0.509597 11.00000 -1.20000 AFIX 0 C21 1 0.282892 0.673782 0.470428 11.00000 0.02733 0.02420 = 0.03491 0.00326 0.00957 0.00314 C22 1 0.005497 0.396660 0.337124 11.00000 0.02683 0.03440 = 0.02994 0.00275 0.00752 0.00479 AFIX 23 H22A 2 -0.036616 0.305266 0.350656 11.00000 -1.20000 H22B 2 -0.087133 0.456983 0.326224 11.00000 -1.20000 AFIX 0 C23 1 0.163216 0.253290 0.255062 11.00000 0.02904 0.02725 = 0.03512 -0.00051 0.00361 0.00408 C24 1 0.236071 0.239666 0.177474 11.00000 0.02708 0.02470 = 0.03591 0.00577 0.00296 0.00213 C25 1 0.298078 0.108538 0.154030 11.00000 0.03374 0.02259 = 0.04057 0.00519 0.00412 0.00422 AFIX 43 H25 2 0.297041 0.032935 0.186804 11.00000 -1.20000 AFIX 0 C26 1 0.361031 0.093621 0.081026 11.00000 0.03447 0.02574 = 0.04224 -0.00255 0.00570 0.00745 AFIX 43 H26 2 0.402186 0.007496 0.063682 11.00000 -1.20000 AFIX 0 C27 1 0.361618 0.208596 0.034553 11.00000 0.03196 0.03145 = 0.03470 -0.00025 0.00711 0.00418 AFIX 43 H27 2 0.404276 0.198385 -0.014341 11.00000 -1.20000 AFIX 0 C28 1 0.240408 0.349261 0.127075 11.00000 0.03458 0.02566 = 0.03467 0.00498 0.00701 0.00311 AFIX 43 H28 2 0.198213 0.436042 0.142497 11.00000 -1.20000 AFIX 0 O8 5 0.411832 0.731692 0.109965 11.00000 0.04234 0.07610 = 0.04244 0.01219 0.01079 0.00647 AFIX 3 H8 2 0.307523 0.746962 0.115745 11.00000 -1.50000 AFIX 0 C29 1 0.480841 0.709693 0.189386 11.00000 0.03849 0.07210 = 0.04795 0.01001 0.00452 0.00787 AFIX 137 H29A 2 0.592576 0.682385 0.189077 11.00000 -1.50000 H29B 2 0.418666 0.635653 0.210032 11.00000 -1.50000 H29C 2 0.478076 0.796123 0.222905 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1 in P1 New: New: P-1 REM R1 = 0.0608 for 3622 Fo > 4sig(Fo) and 0.0734 for all 4296 data REM 371 parameters refined using 0 restraints END WGHT 0.0906 0.9131 REM Highest difference peak 1.541, deepest hole -0.767, 1-sigma level 0.153 Q1 1 0.1175 0.5061 1.0140 11.00000 0.05 1.54 Q2 1 0.0000 0.5000 1.0000 10.50000 0.05 1.41 Q3 1 0.2860 0.5034 1.0367 11.00000 0.05 1.35 Q4 1 0.4734 0.4976 0.9919 11.00000 0.05 1.14 Q5 1 0.2501 0.4853 0.9115 11.00000 0.05 0.68 Q6 1 -0.0284 0.3821 1.0013 11.00000 0.05 0.60 Q7 1 0.4866 0.5982 0.0629 11.00000 0.05 0.50 Q8 1 0.2255 0.3008 0.9011 11.00000 0.05 0.46 Q9 1 0.6824 0.7253 0.1345 11.00000 0.05 0.45 Q10 1 0.6061 0.7490 0.1209 11.00000 0.05 0.43 Q11 1 -0.0258 0.1928 0.2810 11.00000 0.05 0.43 Q12 1 0.4438 0.6020 0.4957 11.00000 0.05 0.42 Q13 1 0.0973 0.0887 0.1566 11.00000 0.05 0.41 Q14 1 0.5265 0.8354 0.6910 11.00000 0.05 0.40 Q15 1 0.3684 0.8173 0.4432 11.00000 0.05 0.40 Q16 1 0.1290 0.9076 0.8369 11.00000 0.05 0.40 Q17 1 0.1528 0.3572 0.9328 11.00000 0.05 0.39 Q18 1 0.4109 0.2806 0.1657 11.00000 0.05 0.38 Q19 1 0.1162 0.5449 0.4151 11.00000 0.05 0.37 Q20 1 0.0506 0.3146 0.0795 11.00000 0.05 0.37 ; _shelx_res_checksum 1940 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_L1@173K _database_code_depnum_ccdc_archive 'CCDC 1413537' _audit_update_record ; 2015-07-17 deposited with the CCDC. 2017-07-31 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic 'anthracene-9,10-diylbil(methylene) dinicotinate' _chemical_name_common ? _chemical_formula_moiety 'C28 H20 N2 O4' _chemical_formula_sum 'C28 H20 N2 O4' _chemical_melting_point ? _exptl_crystal_description needle _exptl_crystal_colour Yellow _diffrn_ambient_temperature 173(2) _chemical_formula_weight 448.46 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.8200(5) _cell_length_b 9.3530(10) _cell_length_c 11.7820(12) _cell_angle_alpha 99.589(8) _cell_angle_beta 99.411(8) _cell_angle_gamma 90.265(8) _cell_volume 516.40(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2610 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.04 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_F_000 234 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.170 _exptl_absorpt_coefficient_mu 0.098 _shelx_estimated_absorpt_T_min 0.964 _shelx_estimated_absorpt_T_max 0.984 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3568 _diffrn_reflns_av_unetI/netI 0.0773 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.778 _diffrn_reflns_theta_max 24.995 _diffrn_reflns_theta_full 24.995 _diffrn_measured_fraction_theta_max 0.953 _diffrn_measured_fraction_theta_full 0.953 _diffrn_reflns_Laue_measured_fraction_max 0.953 _diffrn_reflns_Laue_measured_fraction_full 0.953 _diffrn_reflns_point_group_measured_fraction_max 0.953 _diffrn_reflns_point_group_measured_fraction_full 0.953 _reflns_number_total 1735 _reflns_number_gt 1101 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'X-Area (Stoe & Cie, 2009)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2009)' _computing_data_reduction 'X-RED32(Stoe & Cie, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1735 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.7620(3) 0.25122(16) 0.79707(13) 0.0243(4) Uani 1 1 d . . . . . O2 O 0.5736(4) 0.07680(18) 0.64840(14) 0.0346(5) Uani 1 1 d . . . . . C3 C 1.0752(5) 0.2353(2) 0.4335(2) 0.0265(6) Uani 1 1 d . . . . . H3 H 1.0734 0.1938 0.3541 0.032 Uiso 1 1 calc R U . . . C2 C 1.2526(5) 0.3516(2) 0.4864(2) 0.0271(6) Uani 1 1 d . . . . . H2 H 1.3708 0.3894 0.4406 0.033 Uiso 1 1 calc R U . . . N1 N 1.2698(4) 0.4150(2) 0.59814(18) 0.0286(5) Uani 1 1 d . . . . . C1 C 1.0996(5) 0.3592(2) 0.6600(2) 0.0241(6) Uani 1 1 d . . . . . H1 H 1.1072 0.4020 0.7395 0.029 Uiso 1 1 calc R U . . . C5 C 0.9129(5) 0.2426(2) 0.61473(19) 0.0209(5) Uani 1 1 d . . . . . C4 C 0.8991(5) 0.1802(2) 0.4989(2) 0.0248(6) Uani 1 1 d . . . . . H4 H 0.7715 0.1011 0.4649 0.030 Uiso 1 1 calc R U . . . C6 C 0.7311(5) 0.1802(2) 0.6856(2) 0.0224(6) Uani 1 1 d . . . . . C7 C 0.6164(5) 0.1859(2) 0.8758(2) 0.0244(6) Uani 1 1 d . . . . . H7A H 0.4487 0.1290 0.8307 0.029 Uiso 1 1 calc R U . . . H7B H 0.5526 0.2630 0.9332 0.029 Uiso 1 1 calc R U . . . C13 C 1.0784(5) 0.3076(2) 1.0526(2) 0.0244(6) Uani 1 1 d . . . . . H13 H 0.9538 0.3678 1.0123 0.029 Uiso 1 1 calc R U . . . C14 C 1.0360(5) 0.1528(2) 1.02419(19) 0.0204(5) Uani 1 1 d . . . . . C8 C 0.8113(5) 0.0879(2) 0.93887(18) 0.0204(5) Uani 1 1 d . . . . . C9 C 0.7714(5) -0.0642(2) 0.91355(19) 0.0205(5) Uani 1 1 d . . . . . C10 C 0.5484(5) -0.1373(2) 0.82775(19) 0.0246(6) Uani 1 1 d . . . . . H10 H 0.4175 -0.0809 0.7863 0.030 Uiso 1 1 calc R U . . . C11 C 0.5171(5) -0.2832(2) 0.8036(2) 0.0261(6) Uani 1 1 d . . . . . H11 H 0.3670 -0.3278 0.7458 0.031 Uiso 1 1 calc R U . . . C12 C 0.7074(5) -0.3693(3) 0.8642(2) 0.0272(6) Uani 1 1 d . . . . . H12 H 0.6852 -0.4720 0.8466 0.033 Uiso 1 1 calc R U . . . 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 O1 0.0320(10) 0.0203(8) 0.0214(8) 0.0029(7) 0.0074(7) -0.0035(7) O2 0.0417(12) 0.0330(10) 0.0271(10) -0.0005(8) 0.0062(8) -0.0174(9) C3 0.0277(15) 0.0286(14) 0.0233(12) 0.0038(10) 0.0052(11) 0.0035(11) C2 0.0253(14) 0.0281(13) 0.0300(14) 0.0088(11) 0.0070(12) -0.0001(11) N1 0.0286(12) 0.0251(10) 0.0320(11) 0.0026(9) 0.0076(10) -0.0057(9) C1 0.0236(14) 0.0221(13) 0.0266(13) 0.0035(10) 0.0051(11) 0.0015(10) C5 0.0205(13) 0.0182(11) 0.0241(12) 0.0057(9) 0.0019(10) 0.0032(9) C4 0.0244(14) 0.0211(12) 0.0276(13) 0.0024(10) 0.0021(11) -0.0010(10) C6 0.0244(13) 0.0161(12) 0.0250(13) 0.0002(10) 0.0024(11) -0.0007(10) C7 0.0258(13) 0.0239(12) 0.0257(13) 0.0027(10) 0.0120(11) -0.0026(10) C13 0.0300(14) 0.0193(12) 0.0263(13) 0.0023(10) 0.0134(11) -0.0006(10) C14 0.0237(14) 0.0200(11) 0.0206(12) 0.0030(9) 0.0131(11) -0.0003(10) C8 0.0240(14) 0.0183(11) 0.0206(12) 0.0011(9) 0.0108(10) -0.0008(10) C9 0.0248(13) 0.0200(12) 0.0189(11) 0.0003(9) 0.0130(10) -0.0035(10) C10 0.0275(14) 0.0274(13) 0.0201(12) 0.0029(10) 0.0086(11) -0.0050(11) C11 0.0303(15) 0.0240(13) 0.0234(12) -0.0004(10) 0.0077(11) -0.0090(11) C12 0.0367(16) 0.0172(12) 0.0283(13) -0.0011(10) 0.0121(12) -0.0056(11) _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 O1 C6 1.354(3) . ? O1 C7 1.458(3) . ? O2 C6 1.203(3) . ? C3 C2 1.376(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C2 N1 1.340(3) . ? C2 H2 0.9500 . ? N1 C1 1.340(3) . ? C1 C5 1.387(3) . ? C1 H1 0.9500 . ? C5 C4 1.383(3) . ? C5 C6 1.484(3) . ? C4 H4 0.9500 . ? C7 C8 1.510(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C13 C12 1.355(3) 2_757 ? C13 C14 1.436(3) . ? C13 H13 0.9500 . ? C14 C8 1.410(3) . ? C14 C9 1.440(3) 2_757 ? C8 C9 1.410(3) . ? C9 C10 1.433(3) . ? C9 C14 1.440(3) 2_757 ? C10 C11 1.350(3) . ? C10 H10 0.9500 . ? C11 C12 1.408(4) . ? C11 H11 0.9500 . ? C12 C13 1.355(3) 2_757 ? C12 H12 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 C6 O1 C7 116.14(17) . . ? C2 C3 C4 118.4(2) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? N1 C2 C3 124.3(2) . . ? N1 C2 H2 117.8 . . ? C3 C2 H2 117.8 . . ? C1 N1 C2 116.3(2) . . ? N1 C1 C5 123.8(2) . . ? N1 C1 H1 118.1 . . ? C5 C1 H1 118.1 . . ? C4 C5 C1 118.5(2) . . ? C4 C5 C6 118.5(2) . . ? C1 C5 C6 122.9(2) . . ? C5 C4 C3 118.6(2) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? O2 C6 O1 123.3(2) . . ? O2 C6 C5 123.7(2) . . ? O1 C6 C5 112.98(19) . . ? O1 C7 C8 109.9(2) . . ? O1 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? O1 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C12 C13 C14 121.2(2) 2_757 . ? C12 C13 H13 119.4 2_757 . ? C14 C13 H13 119.4 . . ? C8 C14 C13 121.5(2) . . ? C8 C14 C9 120.28(19) . 2_757 ? C13 C14 C9 118.2(2) . 2_757 ? C14 C8 C9 120.6(2) . . ? C14 C8 C7 118.10(19) . . ? C9 C8 C7 121.3(2) . . ? C8 C9 C10 123.5(2) . . ? C8 C9 C14 119.1(2) . 2_757 ? C10 C9 C14 117.4(2) . 2_757 ? C11 C10 C9 122.5(2) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C12 119.9(2) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 120.9(2) 2_757 . ? C13 C12 H12 119.6 2_757 . ? C11 C12 H12 119.6 . . ? _refine_diff_density_max 0.209 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.052 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL 112 CELL 0.71073 4.8200 9.3530 11.7820 99.589 99.411 90.265 ZERR 1.00 0.0005 0.0010 0.0012 0.008 0.008 0.008 LATT 1 SFAC C H N O UNIT 28 20 2 4 MERG 2 OMIT 0.00 50.00 OMIT 1 -10 1 OMIT 1 9 4 OMIT 3 5 7 FMAP 2 PLAN 5 SIZE 0.170 0.280 0.380 ACTA BOND $H L.S. 50 TEMP -100.00 WGHT 0.045200 FVAR 1.21489 O1 4 0.762035 0.251222 0.797074 11.00000 0.03199 0.02026 = 0.02138 0.00290 0.00742 -0.00345 O2 4 0.573603 0.076805 0.648404 11.00000 0.04172 0.03301 = 0.02711 -0.00049 0.00621 -0.01737 C3 1 1.075211 0.235336 0.433525 11.00000 0.02769 0.02858 = 0.02330 0.00382 0.00522 0.00352 AFIX 43 H3 2 1.073407 0.193835 0.354111 11.00000 -1.20000 AFIX 0 C2 1 1.252614 0.351559 0.486356 11.00000 0.02531 0.02809 = 0.03004 0.00878 0.00696 -0.00012 AFIX 43 H2 2 1.370796 0.389392 0.440597 11.00000 -1.20000 AFIX 0 N1 3 1.269751 0.414960 0.598142 11.00000 0.02859 0.02510 = 0.03202 0.00264 0.00765 -0.00569 C1 1 1.099564 0.359205 0.660049 11.00000 0.02358 0.02208 = 0.02660 0.00351 0.00509 0.00146 AFIX 43 H1 2 1.107213 0.401984 0.739549 11.00000 -1.20000 AFIX 0 C5 1 0.912883 0.242629 0.614733 11.00000 0.02049 0.01817 = 0.02406 0.00575 0.00192 0.00318 C4 1 0.899059 0.180180 0.498926 11.00000 0.02445 0.02114 = 0.02758 0.00237 0.00214 -0.00102 AFIX 43 H4 2 0.771487 0.101097 0.464852 11.00000 -1.20000 AFIX 0 C6 1 0.731147 0.180182 0.685610 11.00000 0.02440 0.01611 = 0.02503 0.00018 0.00237 -0.00069 C7 1 0.616424 0.185865 0.875805 11.00000 0.02579 0.02387 = 0.02568 0.00275 0.01201 -0.00258 AFIX 23 H7A 2 0.448658 0.129008 0.830744 11.00000 -1.20000 H7B 2 0.552641 0.262970 0.933245 11.00000 -1.20000 AFIX 0 C13 1 1.078355 0.307593 1.052572 11.00000 0.02996 0.01930 = 0.02629 0.00226 0.01337 -0.00059 AFIX 43 H13 2 0.953805 0.367833 1.012257 11.00000 -1.20000 AFIX 0 C14 1 1.036013 0.152841 1.024190 11.00000 0.02374 0.02000 = 0.02061 0.00297 0.01315 -0.00027 C8 1 0.811255 0.087940 0.938874 11.00000 0.02399 0.01833 = 0.02064 0.00112 0.01078 -0.00078 C9 1 0.771424 -0.064234 0.913547 11.00000 0.02482 0.01999 = 0.01886 0.00027 0.01299 -0.00348 C10 1 0.548357 -0.137287 0.827752 11.00000 0.02753 0.02743 = 0.02009 0.00293 0.00863 -0.00496 AFIX 43 H10 2 0.417541 -0.080899 0.786293 11.00000 -1.20000 AFIX 0 C11 1 0.517117 -0.283236 0.803626 11.00000 0.03033 0.02402 = 0.02337 -0.00040 0.00770 -0.00900 AFIX 43 H11 2 0.367005 -0.327845 0.745849 11.00000 -1.20000 AFIX 0 C12 1 0.707398 -0.369269 0.864239 11.00000 0.03671 0.01715 = 0.02831 -0.00110 0.01213 -0.00556 AFIX 43 H12 2 0.685217 -0.471964 0.846551 11.00000 -1.20000 AFIX 0 HKLF 4 REM 112 REM R1 = 0.0466 for 1101 Fo > 4sig(Fo) and 0.0895 for all 1735 data REM 154 parameters refined using 0 restraints END WGHT 0.0449 0.0000 REM Highest difference peak 0.209, deepest hole -0.193, 1-sigma level 0.052 Q1 1 0.7038 -0.1039 0.8516 11.00000 0.05 0.21 Q2 1 1.2151 0.5679 0.5826 11.00000 0.05 0.17 Q3 1 1.0142 0.3628 0.9564 11.00000 0.05 0.16 Q4 1 1.1455 0.5215 0.8042 11.00000 0.05 0.15 Q5 1 1.0114 0.3992 0.9074 11.00000 0.05 0.15 ; _shelx_res_checksum 33587 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration . _exptl_crystal_preparation Luminescent ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_AgNO3_dinicoAnthra_Ethanol _database_code_depnum_ccdc_archive 'CCDC 1547595' _audit_update_record ; 2017-05-03 deposited with the CCDC. 2017-07-31 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C28 H20 Ag N2 O4, N O3, C2 H6 O' _chemical_formula_sum 'C30 H26 Ag N3 O8' _exptl_crystal_recrystallization_method 'DCM and Ethanol' _chemical_melting_point ? _exptl_crystal_description 'square plate' _exptl_crystal_colour yellow _diffrn_ambient_temperature 250(2) _chemical_formula_weight 664.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.331(3) _cell_length_b 12.208(4) _cell_length_c 14.076(4) _cell_angle_alpha 97.35(2) _cell_angle_beta 105.78(3) _cell_angle_gamma 97.30(3) _cell_volume 1346.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 5104 _cell_measurement_theta_min 1.52 _cell_measurement_theta_max 25.63 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_F_000 676 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.107 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 0.808 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8049 _exptl_absorpt_correction_T_max 0.9888 _exptl_absorpt_process_details ; Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17261 _diffrn_reflns_av_unetI/netI 0.1127 _diffrn_reflns_av_R_equivalents 0.1309 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.707 _diffrn_reflns_theta_max 25.326 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_point_group_measured_fraction_full 0.985 _reflns_number_total 4784 _reflns_number_gt 1993 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'X-Area (Stoe & Cie, 2009)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2009)' _computing_data_reduction 'X-RED32(Stoe & Cie, 2009)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4784 _refine_ls_number_parameters 381 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.1428 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.871 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.23866(10) -0.01744(5) -0.01467(4) 0.1046(3) Uani 1 1 d . . . . . O2 O 0.6959(5) 0.2119(3) 0.3248(2) 0.0531(11) Uani 1 1 d . . . . . O3 O 0.7659(5) 0.7750(3) 0.6331(2) 0.0544(11) Uani 1 1 d . . . . . O1 O 0.7077(6) 0.1329(3) 0.4609(3) 0.0761(15) Uani 1 1 d . . . . . O4 O 0.7675(6) 0.8665(3) 0.5062(3) 0.0799(15) Uani 1 1 d . . . . . N2 N 1.1407(7) 1.0071(4) 0.8320(3) 0.0617(15) Uani 1 1 d . . . . . N1 N 0.3159(7) -0.0264(4) 0.1433(3) 0.0658(15) Uani 1 1 d . . . . . C5 C 0.5088(7) 0.0468(4) 0.3064(4) 0.0452(14) Uani 1 1 d . . . . . C8 C 0.7887(7) 0.3987(4) 0.4292(4) 0.0464(15) Uani 1 1 d . . . . . C9 C 0.8299(7) 0.4245(4) 0.5339(4) 0.0467(15) Uani 1 1 d . . . . . C15 C 0.6931(7) 0.5925(4) 0.5182(4) 0.0500(16) Uani 1 1 d . . . . . C24 C 0.9550(7) 0.9435(4) 0.6672(4) 0.0453(15) Uani 1 1 d . . . . . C6 C 0.6473(7) 0.1325(4) 0.3733(4) 0.0475(15) Uani 1 1 d . . . . . C1 C 0.4378(8) 0.0536(4) 0.2063(4) 0.0557(17) Uani 1 1 d . . . . . H1 H 0.4766 0.1166 0.1816 0.067 Uiso 1 1 calc R U . . . C25 C 1.0167(8) 1.0401(4) 0.6382(4) 0.0523(16) Uani 1 1 d . . . . . H25 H 0.9732 1.0521 0.5721 0.063 Uiso 1 1 calc R U . . . C28 C 1.0207(8) 0.9302(5) 0.7650(4) 0.0549(16) Uani 1 1 d . . . . . H28 H 0.9799 0.8647 0.7857 0.066 Uiso 1 1 calc R U . . . C14 C 0.7789(7) 0.5226(4) 0.5784(4) 0.0496(16) Uani 1 1 d . . . . . C16 C 0.6568(7) 0.5680(4) 0.4133(4) 0.0508(16) Uani 1 1 d . . . . . N3 N 0.3796(11) -0.2446(6) -0.0243(5) 0.090(2) Uani 1 1 d . U . . . C10 C 0.9176(8) 0.3576(5) 0.6001(4) 0.0575(17) Uani 1 1 d . . . . . H10 H 0.9493 0.2922 0.5729 0.069 Uiso 1 1 calc R U . . . C4 C 0.4483(8) -0.0451(4) 0.3414(4) 0.0533(16) Uani 1 1 d . . . . . H4 H 0.4925 -0.0523 0.4088 0.064 Uiso 1 1 calc R U . . . C23 C 0.8214(8) 0.8594(4) 0.5939(4) 0.0509(15) Uani 1 1 d . . . . . C21 C 0.7043(7) 0.4681(5) 0.3687(4) 0.0497(16) Uani 1 1 d . . . . . C26 C 1.1410(8) 1.1182(4) 0.7055(4) 0.0566(17) Uani 1 1 d . . . . . H26 H 1.1850 1.1839 0.6863 0.068 Uiso 1 1 calc R U . . . C12 C 0.9063(9) 0.4812(5) 0.7444(4) 0.0656(19) Uani 1 1 d . . . . . H12 H 0.9321 0.4995 0.8144 0.079 Uiso 1 1 calc R U . . . C13 C 0.8214(8) 0.5464(5) 0.6854(4) 0.0577(17) Uani 1 1 d . . . . . H13 H 0.7889 0.6097 0.7156 0.069 Uiso 1 1 calc R U . . . C2 C 0.2602(8) -0.1144(4) 0.1801(4) 0.0596(17) Uani 1 1 d . . . . . H2 H 0.1739 -0.1704 0.1369 0.071 Uiso 1 1 calc R U . . . C27 C 1.2010(8) 1.0985(5) 0.8028(4) 0.0632(18) Uani 1 1 d . . . . . H27 H 1.2871 1.1517 0.8494 0.076 Uiso 1 1 calc R U . . . C17 C 0.5754(8) 0.6365(5) 0.3481(4) 0.0602(18) Uani 1 1 d . . . . . H17 H 0.5464 0.7026 0.3760 0.072 Uiso 1 1 calc R U . . . C3 C 0.3231(8) -0.1264(5) 0.2772(4) 0.0577(17) Uani 1 1 d . . . . . H3 H 0.2811 -0.1898 0.3003 0.069 Uiso 1 1 calc R U . . . C7 C 0.8413(8) 0.2989(4) 0.3803(4) 0.0571(17) Uani 1 1 d . . . . . H7A H 0.9032 0.3225 0.3342 0.069 Uiso 1 1 calc R U . . . H7B H 0.9182 0.2675 0.4317 0.069 Uiso 1 1 calc R U . . . C19 C 0.5814(9) 0.5125(6) 0.2038(5) 0.072(2) Uani 1 1 d . . . . . H19 H 0.5533 0.4939 0.1337 0.087 Uiso 1 1 calc R U . . . C22 C 0.6295(8) 0.6877(4) 0.5680(4) 0.0582(17) Uani 1 1 d . . . . . H22A H 0.5575 0.7212 0.5161 0.070 Uiso 1 1 calc R U . . . H22B H 0.5597 0.6579 0.6078 0.070 Uiso 1 1 calc R U . . . C11 C 0.9563(8) 0.3857(5) 0.7010(5) 0.0633(19) Uani 1 1 d . . . . . H11 H 1.0172 0.3411 0.7424 0.076 Uiso 1 1 calc R U . . . C20 C 0.6639(8) 0.4439(5) 0.2617(4) 0.0644(19) Uani 1 1 d . . . . . H20 H 0.6946 0.3800 0.2312 0.077 Uiso 1 1 calc R U . . . C18 C 0.5374(9) 0.6107(6) 0.2467(5) 0.073(2) Uani 1 1 d . . . . . H18 H 0.4824 0.6579 0.2057 0.088 Uiso 1 1 calc R U . . . O5 O 0.4780(9) -0.1596(6) -0.0184(5) 0.131(2) Uani 1 1 d . U . . . O6 O 0.2386(10) -0.2499(7) -0.0796(6) 0.168(3) Uani 1 1 d . U . . . C30 C -0.1232(16) -0.3710(6) 0.0256(7) 0.142(4) Uani 1 1 d . U . . . H30A H -0.0005 -0.3598 0.0473 0.213 Uiso 1 1 calc R U . . . H30B H -0.1675 -0.4494 -0.0022 0.213 Uiso 1 1 calc R U . . . H30C H -0.1640 -0.3495 0.0825 0.213 Uiso 1 1 calc R U . . . O8 O -0.0967(15) -0.2052(6) -0.0544(7) 0.189(4) Uani 1 1 d . U . . . H8 H -0.0181 -0.2166 -0.0781 0.284 Uiso 1 1 calc R U . . . O7 O 0.4311(16) -0.3134(7) 0.0188(6) 0.209(5) Uani 1 1 d . U . . . C29 C -0.1862(13) -0.2949(9) -0.0591(7) 0.124(3) Uani 1 1 d . U . . . H29A H -0.2013 -0.3402 -0.1246 0.149 Uiso 1 1 calc R U . . . H29B H -0.2980 -0.2794 -0.0573 0.149 Uiso 1 1 calc R U . . . 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 0.1458(6) 0.0874(4) 0.0455(3) 0.0136(2) -0.0158(3) -0.0135(4) O2 0.061(3) 0.045(2) 0.046(2) 0.0000(18) 0.0157(19) -0.0077(19) O3 0.069(3) 0.0404(19) 0.048(2) 0.0054(17) 0.0148(19) -0.0055(19) O1 0.091(4) 0.062(2) 0.049(2) 0.011(2) -0.009(2) -0.018(2) O4 0.093(4) 0.072(3) 0.047(2) 0.015(2) -0.009(2) -0.026(2) N2 0.078(4) 0.049(3) 0.047(3) 0.007(2) 0.004(3) 0.001(3) N1 0.077(4) 0.055(3) 0.050(3) 0.002(3) 0.004(3) -0.006(3) C5 0.051(4) 0.040(3) 0.042(3) 0.005(3) 0.014(3) 0.001(3) C8 0.042(4) 0.040(3) 0.050(3) -0.004(3) 0.013(3) -0.007(3) C9 0.037(4) 0.040(3) 0.057(3) 0.002(3) 0.012(3) -0.006(3) C15 0.047(4) 0.039(3) 0.056(3) 0.000(3) 0.013(3) -0.009(3) C24 0.053(4) 0.040(3) 0.038(3) 0.004(2) 0.010(3) 0.000(3) C6 0.055(4) 0.036(3) 0.044(3) 0.002(3) 0.007(3) 0.001(3) C1 0.066(4) 0.046(3) 0.045(3) 0.007(3) 0.008(3) -0.009(3) C25 0.061(4) 0.049(3) 0.047(3) 0.016(3) 0.015(3) 0.006(3) C28 0.067(4) 0.045(3) 0.046(3) 0.011(3) 0.008(3) 0.001(3) C14 0.044(4) 0.049(3) 0.050(3) 0.011(3) 0.012(3) -0.011(3) C16 0.046(4) 0.047(3) 0.049(3) 0.006(3) 0.006(3) -0.012(3) N3 0.108(6) 0.086(4) 0.071(4) 0.007(4) 0.027(4) 0.008(4) C10 0.056(4) 0.044(3) 0.062(4) 0.002(3) 0.009(3) -0.006(3) C4 0.057(4) 0.054(3) 0.045(3) 0.012(3) 0.011(3) 0.002(3) C23 0.056(4) 0.042(3) 0.054(3) 0.012(3) 0.016(3) 0.002(3) C21 0.045(4) 0.046(3) 0.048(3) 0.001(3) 0.009(3) -0.012(3) C26 0.062(4) 0.048(3) 0.053(3) 0.008(3) 0.011(3) -0.005(3) C12 0.085(5) 0.058(4) 0.049(3) 0.008(3) 0.021(3) -0.005(4) C13 0.069(5) 0.046(3) 0.056(4) 0.007(3) 0.020(3) -0.001(3) C2 0.067(5) 0.042(3) 0.058(4) 0.001(3) 0.008(3) -0.003(3) C27 0.071(5) 0.053(3) 0.051(3) 0.000(3) 0.003(3) -0.005(3) C17 0.056(4) 0.051(3) 0.062(4) 0.009(3) 0.004(3) -0.001(3) C3 0.057(4) 0.049(3) 0.059(4) 0.010(3) 0.010(3) -0.005(3) C7 0.050(4) 0.051(3) 0.064(4) 0.001(3) 0.017(3) -0.008(3) C19 0.074(5) 0.075(4) 0.055(4) 0.015(4) 0.007(3) -0.012(4) C22 0.057(4) 0.052(3) 0.060(3) 0.010(3) 0.015(3) -0.008(3) C11 0.066(5) 0.050(4) 0.065(4) 0.013(3) 0.008(3) -0.002(3) C20 0.064(5) 0.062(4) 0.056(4) -0.002(3) 0.018(3) -0.019(3) C18 0.069(5) 0.071(4) 0.066(4) 0.022(4) 0.005(3) -0.015(4) O5 0.130(6) 0.127(5) 0.124(5) 0.015(4) 0.037(4) -0.016(4) O6 0.111(6) 0.180(7) 0.168(7) -0.049(5) 0.004(5) 0.015(5) C30 0.244(13) 0.068(5) 0.139(8) 0.031(5) 0.094(8) 0.021(6) O8 0.275(13) 0.129(5) 0.166(7) 0.069(5) 0.063(7) -0.001(6) O7 0.358(14) 0.155(6) 0.163(7) 0.097(6) 0.104(7) 0.089(7) C29 0.097(7) 0.149(8) 0.106(6) -0.019(6) 0.031(5) -0.013(6) _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 2.161(5) . ? Ag1 N2 2.165(4) 1_444 ? O2 C6 1.338(6) . ? O2 C7 1.467(6) . ? O3 C23 1.321(6) . ? O3 C22 1.463(6) . ? O1 C6 1.198(6) . ? O4 C23 1.212(6) . ? N2 C27 1.324(7) . ? N2 C28 1.338(6) . ? N2 Ag1 2.165(4) 1_666 ? N1 C2 1.336(7) . ? N1 C1 1.344(6) . ? C5 C4 1.374(7) . ? C5 C1 1.390(7) . ? C5 C6 1.470(7) . ? C8 C21 1.396(8) . ? C8 C9 1.403(7) . ? C8 C7 1.496(8) . ? C9 C10 1.430(8) . ? C9 C14 1.446(8) . ? C15 C14 1.402(8) . ? C15 C16 1.408(8) . ? C15 C22 1.507(9) . ? C24 C28 1.376(7) . ? C24 C25 1.380(7) . ? C24 C23 1.473(7) . ? C1 H1 0.9400 . ? C25 C26 1.365(7) . ? C25 H25 0.9400 . ? C28 H28 0.9400 . ? C14 C13 1.432(8) . ? C16 C17 1.416(8) . ? C16 C21 1.449(9) . ? N3 O7 1.157(9) . ? N3 O6 1.208(9) . ? N3 O5 1.217(8) . ? C10 C11 1.355(8) . ? C10 H10 0.9400 . ? C4 C3 1.373(7) . ? C4 H4 0.9400 . ? C21 C20 1.433(8) . ? C26 C27 1.388(8) . ? C26 H26 0.9400 . ? C12 C13 1.347(8) . ? C12 C11 1.410(9) . ? C12 H12 0.9400 . ? C13 H13 0.9400 . ? C2 C3 1.359(7) . ? C2 H2 0.9400 . ? C27 H27 0.9400 . ? C17 C18 1.361(8) . ? C17 H17 0.9400 . ? C3 H3 0.9400 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C19 C20 1.361(9) . ? C19 C18 1.408(10) . ? C19 H19 0.9400 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C11 H11 0.9400 . ? C20 H20 0.9400 . ? C18 H18 0.9400 . ? C30 C29 1.621(13) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? O8 C29 1.227(9) . ? O8 H8 0.8300 . ? C29 H29A 0.9800 . ? C29 H29B 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 N2 172.4(2) . 1_444 ? C6 O2 C7 117.8(4) . . ? C23 O3 C22 118.3(4) . . ? C27 N2 C28 119.0(5) . . ? C27 N2 Ag1 120.1(4) . 1_666 ? C28 N2 Ag1 120.9(3) . 1_666 ? C2 N1 C1 117.9(5) . . ? C2 N1 Ag1 122.5(4) . . ? C1 N1 Ag1 119.2(4) . . ? C4 C5 C1 117.7(5) . . ? C4 C5 C6 120.2(5) . . ? C1 C5 C6 122.0(5) . . ? C21 C8 C9 120.8(5) . . ? C21 C8 C7 118.6(5) . . ? C9 C8 C7 120.5(5) . . ? C8 C9 C10 123.6(6) . . ? C8 C9 C14 118.9(5) . . ? C10 C9 C14 117.5(5) . . ? C14 C15 C16 120.1(6) . . ? C14 C15 C22 118.3(5) . . ? C16 C15 C22 121.4(6) . . ? C28 C24 C25 118.0(5) . . ? C28 C24 C23 122.4(5) . . ? C25 C24 C23 119.6(5) . . ? O1 C6 O2 123.8(5) . . ? O1 C6 C5 124.5(5) . . ? O2 C6 C5 111.7(4) . . ? N1 C1 C5 122.7(5) . . ? N1 C1 H1 118.7 . . ? C5 C1 H1 118.7 . . ? C26 C25 C24 120.0(5) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? N2 C28 C24 122.4(5) . . ? N2 C28 H28 118.8 . . ? C24 C28 H28 118.8 . . ? C15 C14 C13 121.6(6) . . ? C15 C14 C9 120.7(5) . . ? C13 C14 C9 117.7(5) . . ? C15 C16 C17 123.2(6) . . ? C15 C16 C21 119.2(5) . . ? C17 C16 C21 117.6(5) . . ? O7 N3 O6 126.8(10) . . ? O7 N3 O5 117.7(10) . . ? O6 N3 O5 115.3(9) . . ? C11 C10 C9 121.9(6) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C3 C4 C5 119.6(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? O4 C23 O3 123.0(5) . . ? O4 C23 C24 123.7(5) . . ? O3 C23 C24 113.3(4) . . ? C8 C21 C20 121.4(6) . . ? C8 C21 C16 120.3(5) . . ? C20 C21 C16 118.2(6) . . ? C25 C26 C27 118.5(5) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C13 C12 C11 119.9(6) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 122.4(6) . . ? C12 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? N1 C2 C3 122.7(5) . . ? N1 C2 H2 118.6 . . ? C3 C2 H2 118.6 . . ? N2 C27 C26 122.0(5) . . ? N2 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C18 C17 C16 122.7(7) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? O2 C7 C8 112.0(5) . . ? O2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? O2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C20 C19 C18 121.4(6) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? O3 C22 C15 113.1(5) . . ? O3 C22 H22A 109.0 . . ? C15 C22 H22A 109.0 . . ? O3 C22 H22B 109.0 . . ? C15 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C10 C11 C12 120.6(6) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C19 C20 C21 120.7(7) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C17 C18 C19 119.3(7) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 O8 H8 109.5 . . ? O8 C29 C30 118.3(9) . . ? O8 C29 H29A 107.7 . . ? C30 C29 H29A 107.7 . . ? O8 C29 H29B 107.7 . . ? C30 C29 H29B 107.7 . . ? H29A C29 H29B 107.1 . . ? 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 C21 C8 C9 C10 -179.4(5) . . . . ? C7 C8 C9 C10 -2.1(8) . . . . ? C21 C8 C9 C14 1.8(7) . . . . ? C7 C8 C9 C14 179.1(5) . . . . ? C7 O2 C6 O1 5.6(9) . . . . ? C7 O2 C6 C5 -175.8(5) . . . . ? C4 C5 C6 O1 -5.1(10) . . . . ? C1 C5 C6 O1 176.7(6) . . . . ? C4 C5 C6 O2 176.2(5) . . . . ? C1 C5 C6 O2 -1.9(8) . . . . ? C2 N1 C1 C5 1.1(10) . . . . ? Ag1 N1 C1 C5 -172.0(5) . . . . ? C4 C5 C1 N1 -1.0(10) . . . . ? C6 C5 C1 N1 177.2(6) . . . . ? C28 C24 C25 C26 0.9(9) . . . . ? C23 C24 C25 C26 -179.7(6) . . . . ? C27 N2 C28 C24 -1.3(10) . . . . ? Ag1 N2 C28 C24 179.6(5) 1_666 . . . ? C25 C24 C28 N2 0.1(10) . . . . ? C23 C24 C28 N2 -179.2(6) . . . . ? C16 C15 C14 C13 178.5(5) . . . . ? C22 C15 C14 C13 -6.3(8) . . . . ? C16 C15 C14 C9 -0.5(8) . . . . ? C22 C15 C14 C9 174.7(4) . . . . ? C8 C9 C14 C15 -1.4(8) . . . . ? C10 C9 C14 C15 179.7(5) . . . . ? C8 C9 C14 C13 179.5(5) . . . . ? C10 C9 C14 C13 0.6(7) . . . . ? C14 C15 C16 C17 -178.0(5) . . . . ? C22 C15 C16 C17 7.0(8) . . . . ? C14 C15 C16 C21 2.0(8) . . . . ? C22 C15 C16 C21 -173.0(5) . . . . ? C8 C9 C10 C11 179.4(6) . . . . ? C14 C9 C10 C11 -1.7(8) . . . . ? C1 C5 C4 C3 0.6(9) . . . . ? C6 C5 C4 C3 -177.7(6) . . . . ? C22 O3 C23 O4 -1.8(9) . . . . ? C22 O3 C23 C24 178.3(5) . . . . ? C28 C24 C23 O4 -176.2(7) . . . . ? C25 C24 C23 O4 4.5(10) . . . . ? C28 C24 C23 O3 3.8(9) . . . . ? C25 C24 C23 O3 -175.6(5) . . . . ? C9 C8 C21 C20 179.0(5) . . . . ? C7 C8 C21 C20 1.6(8) . . . . ? C9 C8 C21 C16 -0.3(8) . . . . ? C7 C8 C21 C16 -177.7(5) . . . . ? C15 C16 C21 C8 -1.6(8) . . . . ? C17 C16 C21 C8 178.4(5) . . . . ? C15 C16 C21 C20 179.1(5) . . . . ? C17 C16 C21 C20 -1.0(8) . . . . ? C24 C25 C26 C27 -0.8(10) . . . . ? C11 C12 C13 C14 -0.1(9) . . . . ? C15 C14 C13 C12 -178.8(6) . . . . ? C9 C14 C13 C12 0.2(8) . . . . ? C1 N1 C2 C3 -0.8(10) . . . . ? Ag1 N1 C2 C3 172.1(5) . . . . ? C28 N2 C27 C26 1.5(10) . . . . ? Ag1 N2 C27 C26 -179.4(5) 1_666 . . . ? C25 C26 C27 N2 -0.4(10) . . . . ? C15 C16 C17 C18 -178.4(6) . . . . ? C21 C16 C17 C18 1.6(9) . . . . ? N1 C2 C3 C4 0.4(10) . . . . ? C5 C4 C3 C2 -0.3(10) . . . . ? C6 O2 C7 C8 -91.4(6) . . . . ? C21 C8 C7 O2 -70.3(6) . . . . ? C9 C8 C7 O2 112.3(6) . . . . ? C23 O3 C22 C15 90.7(6) . . . . ? C14 C15 C22 O3 67.6(6) . . . . ? C16 C15 C22 O3 -117.3(5) . . . . ? C9 C10 C11 C12 2.0(9) . . . . ? C13 C12 C11 C10 -1.0(9) . . . . ? C18 C19 C20 C21 1.8(9) . . . . ? C8 C21 C20 C19 180.0(6) . . . . ? C16 C21 C20 C19 -0.7(8) . . . . ? C16 C17 C18 C19 -0.6(10) . . . . ? C20 C19 C18 C17 -1.2(10) . . . . ? 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 O8 H8 O6 0.83 2.23 3.017(15) 157.8 . _refine_diff_density_max 0.609 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.070 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P-1 CELL 0.71073 8.3306 12.2084 14.0757 97.353 105.778 97.302 ZERR 2.00 0.0033 0.0035 0.0038 0.023 0.026 0.028 LATT 1 SFAC C H AG N O UNIT 60 52 2 6 16 MERG 2 OMIT 0 -1 4 OMIT 0 -7 3 OMIT 0 0 1 OMIT 3 -3 11 OMIT 3 -11 1 DELU 0.010 0.010 C30 O8 C29 SIMU 0.040 0.080 1.700 C30 O8 C29 DELU 0.010 0.010 N3 O5 O6 O7 SIMU 0.040 0.080 1.700 N3 O5 O6 O7 HTAB O8 O6 FMAP 2 PLAN 5 ACTA BOND $H CONF LIST 6 L.S. 10 TEMP -23.00 WGHT 0.049800 FVAR 0.38943 AG1 3 0.238660 -0.017442 -0.014674 11.00000 0.14584 0.08738 = 0.04552 0.01361 -0.01578 -0.01351 O2 5 0.695915 0.211909 0.324751 11.00000 0.06142 0.04516 = 0.04599 0.00002 0.01565 -0.00769 O3 5 0.765893 0.774996 0.633077 11.00000 0.06874 0.04038 = 0.04803 0.00545 0.01482 -0.00546 O1 5 0.707725 0.132904 0.460911 11.00000 0.09056 0.06235 = 0.04948 0.01129 -0.00946 -0.01765 O4 5 0.767513 0.866458 0.506161 11.00000 0.09339 0.07197 = 0.04719 0.01516 -0.00858 -0.02558 N2 4 1.140735 1.007141 0.831963 11.00000 0.07808 0.04872 = 0.04668 0.00729 0.00407 0.00053 N1 4 0.315914 -0.026367 0.143292 11.00000 0.07670 0.05503 = 0.05029 0.00247 0.00370 -0.00558 C5 1 0.508771 0.046847 0.306435 11.00000 0.05092 0.04028 = 0.04214 0.00495 0.01385 0.00073 C8 1 0.788708 0.398723 0.429157 11.00000 0.04208 0.03955 = 0.05038 -0.00365 0.01316 -0.00720 C9 1 0.829861 0.424469 0.533919 11.00000 0.03713 0.03968 = 0.05725 0.00180 0.01221 -0.00586 C15 1 0.693099 0.592525 0.518227 11.00000 0.04718 0.03878 = 0.05594 0.00007 0.01300 -0.00918 C24 1 0.955013 0.943493 0.667212 11.00000 0.05290 0.04002 = 0.03800 0.00371 0.00979 0.00032 C6 1 0.647334 0.132526 0.373279 11.00000 0.05487 0.03579 = 0.04449 0.00180 0.00745 0.00122 C1 1 0.437800 0.053566 0.206276 11.00000 0.06572 0.04594 = 0.04533 0.00713 0.00828 -0.00862 AFIX 43 H1 2 0.476641 0.116585 0.181592 11.00000 -1.20000 AFIX 0 C25 1 1.016729 1.040094 0.638184 11.00000 0.06135 0.04885 = 0.04748 0.01626 0.01515 0.00571 AFIX 43 H25 2 0.973174 1.052073 0.572077 11.00000 -1.20000 AFIX 0 C28 1 1.020741 0.930206 0.765048 11.00000 0.06742 0.04518 = 0.04576 0.01072 0.00832 0.00113 AFIX 43 H28 2 0.979887 0.864696 0.785663 11.00000 -1.20000 AFIX 0 C14 1 0.778860 0.522645 0.578408 11.00000 0.04437 0.04892 = 0.04999 0.01052 0.01217 -0.01081 C16 1 0.656802 0.567986 0.413333 11.00000 0.04608 0.04680 = 0.04855 0.00605 0.00568 -0.01179 N3 4 0.379581 -0.244573 -0.024278 11.00000 0.10797 0.08610 = 0.07109 0.00651 0.02668 0.00795 C10 1 0.917587 0.357558 0.600107 11.00000 0.05555 0.04396 = 0.06203 0.00234 0.00862 -0.00621 AFIX 43 H10 2 0.949263 0.292202 0.572858 11.00000 -1.20000 AFIX 0 C4 1 0.448317 -0.045103 0.341401 11.00000 0.05742 0.05379 = 0.04490 0.01198 0.01055 0.00176 AFIX 43 H4 2 0.492463 -0.052279 0.408839 11.00000 -1.20000 AFIX 0 C23 1 0.821450 0.859431 0.593852 11.00000 0.05636 0.04213 = 0.05362 0.01188 0.01625 0.00170 C21 1 0.704271 0.468130 0.368696 11.00000 0.04482 0.04622 = 0.04815 0.00128 0.00934 -0.01162 C26 1 1.141014 1.118225 0.705484 11.00000 0.06203 0.04767 = 0.05273 0.00763 0.01138 -0.00491 AFIX 43 H26 2 1.184964 1.183892 0.686348 11.00000 -1.20000 AFIX 0 C12 1 0.906267 0.481243 0.744388 11.00000 0.08522 0.05761 = 0.04946 0.00759 0.02085 -0.00508 AFIX 43 H12 2 0.932095 0.499464 0.814410 11.00000 -1.20000 AFIX 0 C13 1 0.821404 0.546377 0.685443 11.00000 0.06866 0.04649 = 0.05561 0.00730 0.01979 -0.00050 AFIX 43 H13 2 0.788910 0.609719 0.715642 11.00000 -1.20000 AFIX 0 C2 1 0.260171 -0.114429 0.180061 11.00000 0.06735 0.04189 = 0.05761 0.00147 0.00758 -0.00333 AFIX 43 H2 2 0.173904 -0.170405 0.136945 11.00000 -1.20000 AFIX 0 C27 1 1.201017 1.098541 0.802771 11.00000 0.07067 0.05307 = 0.05058 -0.00004 0.00345 -0.00483 AFIX 43 H27 2 1.287130 1.151740 0.849398 11.00000 -1.20000 AFIX 0 C17 1 0.575413 0.636529 0.348107 11.00000 0.05585 0.05122 = 0.06240 0.00911 0.00374 -0.00148 AFIX 43 H17 2 0.546446 0.702618 0.376028 11.00000 -1.20000 AFIX 0 C3 1 0.323057 -0.126414 0.277238 11.00000 0.05693 0.04922 = 0.05921 0.01003 0.01021 -0.00468 AFIX 43 H3 2 0.281147 -0.189814 0.300297 11.00000 -1.20000 AFIX 0 C7 1 0.841348 0.298853 0.380258 11.00000 0.04995 0.05087 = 0.06374 0.00094 0.01720 -0.00814 AFIX 23 H7A 2 0.903151 0.322466 0.334187 11.00000 -1.20000 H7B 2 0.918163 0.267523 0.431652 11.00000 -1.20000 AFIX 0 C19 1 0.581421 0.512501 0.203828 11.00000 0.07423 0.07468 = 0.05531 0.01461 0.00737 -0.01200 AFIX 43 H19 2 0.553278 0.493900 0.133721 11.00000 -1.20000 AFIX 0 C22 1 0.629529 0.687729 0.567973 11.00000 0.05652 0.05185 = 0.06011 0.00985 0.01478 -0.00830 AFIX 23 H22A 2 0.557488 0.721237 0.516147 11.00000 -1.20000 H22B 2 0.559667 0.657927 0.607765 11.00000 -1.20000 AFIX 0 C11 1 0.956336 0.385718 0.701002 11.00000 0.06578 0.04976 = 0.06530 0.01313 0.00810 -0.00162 AFIX 43 H11 2 1.017159 0.341138 0.742427 11.00000 -1.20000 AFIX 0 C20 1 0.663866 0.443915 0.261723 11.00000 0.06367 0.06197 = 0.05600 -0.00174 0.01753 -0.01913 AFIX 43 H20 2 0.694602 0.380009 0.231204 11.00000 -1.20000 AFIX 0 C18 1 0.537406 0.610670 0.246675 11.00000 0.06898 0.07137 = 0.06551 0.02194 0.00539 -0.01525 AFIX 43 H18 2 0.482355 0.657850 0.205664 11.00000 -1.20000 AFIX 0 O5 5 0.478046 -0.159579 -0.018375 11.00000 0.12980 0.12720 = 0.12434 0.01530 0.03699 -0.01574 O6 5 0.238640 -0.249867 -0.079621 11.00000 0.11066 0.17998 = 0.16774 -0.04902 0.00392 0.01471 C30 1 -0.123238 -0.371042 0.025635 11.00000 0.24389 0.06816 = 0.13877 0.03063 0.09402 0.02054 AFIX 137 H30A 2 -0.000528 -0.359764 0.047319 11.00000 -1.50000 H30B 2 -0.167492 -0.449431 -0.002166 11.00000 -1.50000 H30C 2 -0.164012 -0.349464 0.082451 11.00000 -1.50000 AFIX 0 O8 5 -0.096700 -0.205244 -0.054388 11.00000 0.27475 0.12915 = 0.16579 0.06945 0.06297 -0.00076 AFIX 147 H8 2 -0.018120 -0.216631 -0.078069 11.00000 -1.50000 AFIX 0 O7 5 0.431084 -0.313375 0.018837 11.00000 0.35757 0.15549 = 0.16285 0.09687 0.10365 0.08891 C29 1 -0.186230 -0.294929 -0.059118 11.00000 0.09651 0.14937 = 0.10617 -0.01880 0.03103 -0.01282 AFIX 23 H29A 2 -0.201322 -0.340155 -0.124649 11.00000 -1.20000 H29B 2 -0.297977 -0.279354 -0.057262 11.00000 -1.20000 AFIX 0 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0499 for 1993 Fo > 4sig(Fo) and 0.1428 for all 4784 data REM 381 parameters refined using 39 restraints END WGHT 0.0496 0.0000 REM Highest difference peak 0.609, deepest hole -0.334, 1-sigma level 0.070 Q1 1 -0.1666 -0.3567 0.0596 11.00000 0.05 0.45 Q2 1 -0.1494 -0.4055 0.0008 11.00000 0.05 0.45 Q3 1 0.2462 -0.3263 -0.0031 11.00000 0.05 0.33 Q4 1 -0.2692 -0.2699 -0.1139 11.00000 0.05 0.29 Q5 1 0.4832 -0.3313 0.0405 11.00000 0.05 0.25 ; _shelx_res_checksum 82623 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration .