# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ilb1219_0m _database_code_depnum_ccdc_archive 'CCDC 903738' #TrackingRef '1-EtOH_150K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 Ag4 F28 N6 O10' _chemical_formula_weight 1784.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8667(2) _cell_length_b 12.0846(3) _cell_length_c 15.4595(3) _cell_angle_alpha 109.4510(10) _cell_angle_beta 98.2280(10) _cell_angle_gamma 103.5590(10) _cell_volume 1473.55(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'block from a needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 1.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6859 _exptl_absorpt_correction_T_max 0.6945 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27606 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6757 _reflns_number_gt 6003 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+7.8246P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6757 _refine_ls_number_parameters 405 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1548 _refine_ls_wR_factor_gt 0.1490 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.15096(4) 0.78025(3) 0.80705(2) 0.02964(12) Uani 1 1 d . . . Ag2 Ag 0.67599(5) 0.59576(3) 0.62331(3) 0.03626(13) Uani 1 1 d . . . O1A O 0.9382(6) 0.8364(5) 0.7252(3) 0.0566(12) Uani 1 1 d . . . O1B O 0.6766(4) 0.7986(3) 0.6756(3) 0.0367(8) Uani 1 1 d . . . C1 C 0.8156(6) 0.8650(3) 0.7148(3) 0.0313(10) Uani 1 1 d D A . C2 C 0.8357(5) 1.0040(3) 0.7549(2) 0.0393(11) Uani 1 1 d D . . F2A F 0.9527(7) 1.0627(8) 0.8352(5) 0.067(3) Uiso 0.533(8) 1 d PD A 1 F2B F 0.7029(6) 1.0308(6) 0.7765(5) 0.0485(18) Uiso 0.533(8) 1 d PD A 1 C3 C 0.8096(6) 1.0669(5) 0.6846(3) 0.040(2) Uiso 0.533(8) 1 d PD A 1 F3A F 0.6536(6) 1.0271(6) 0.6393(5) 0.0522(18) Uiso 0.533(8) 1 d PD A 1 F3B F 0.8470(8) 1.1901(5) 0.7293(5) 0.057(2) Uiso 0.533(8) 1 d PD A 1 C4 C 0.9072(8) 1.0462(5) 0.6091(3) 0.042(2) Uiso 0.533(8) 1 d PD A 1 F4A F 0.8906(14) 1.1068(6) 0.5509(5) 0.070(3) Uiso 0.533(8) 1 d PD A 1 F4B F 0.8657(9) 0.9258(5) 0.5533(5) 0.059(2) Uiso 0.533(8) 1 d PD A 1 F4C F 1.0661(8) 1.0817(8) 0.6463(8) 0.095(4) Uiso 0.533(8) 1 d PD A 1 F2Y F 0.9797(7) 1.0724(8) 0.8127(6) 0.046(2) Uiso 0.467(8) 1 d PD A 2 F2Z F 0.7280(7) 1.0260(7) 0.8100(6) 0.0412(18) Uiso 0.467(8) 1 d PD A 2 C3' C 0.8999(8) 1.0721(6) 0.6931(4) 0.055(3) Uiso 0.467(8) 1 d PD A 2 F3Z F 0.9199(11) 1.1940(7) 0.7333(7) 0.069(3) Uiso 0.467(8) 1 d PD A 2 F3Y F 1.0391(10) 1.0614(9) 0.6711(8) 0.072(3) Uiso 0.467(8) 1 d PD A 2 C4' C 0.7888(7) 1.0328(5) 0.5950(4) 0.053(3) Uiso 0.467(8) 1 d PD A 2 F4X F 0.6386(9) 1.0366(8) 0.5973(8) 0.073(3) Uiso 0.467(8) 1 d PD A 2 F4Y F 0.7754(9) 0.9173(5) 0.5373(5) 0.047(2) Uiso 0.467(8) 1 d PD A 2 F4Z F 0.8454(15) 1.1070(6) 0.5507(6) 0.060(3) Uiso 0.467(8) 1 d PD A 2 O11A O 0.4627(4) 0.5004(4) 0.6939(3) 0.0362(8) Uani 1 1 d . B . O11B O 0.7159(4) 0.5434(3) 0.7672(3) 0.0363(8) Uani 1 1 d . B . C11 C 0.5680(5) 0.5026(4) 0.7573(3) 0.0270(9) Uani 1 1 d D . . C12 C 0.5061(8) 0.4476(4) 0.8268(3) 0.034(8) Uiso 0.453(11) 1 d PD B 1 F12A F 0.6037(8) 0.5110(7) 0.9141(5) 0.0339(18) Uiso 0.453(11) 1 d PD B 1 F12B F 0.3606(8) 0.4603(8) 0.8339(6) 0.0353(19) Uiso 0.453(11) 1 d PD B 1 C13 C 0.4959(8) 0.3105(4) 0.7949(3) 0.058(6) Uiso 0.453(11) 1 d PD B 1 F13A F 0.4163(10) 0.2483(8) 0.7035(4) 0.057(3) Uiso 0.453(11) 1 d PD B 1 F13B F 0.6456(8) 0.3014(8) 0.8005(6) 0.048(2) Uiso 0.453(11) 1 d PD B 1 C14 C 0.4304(7) 0.2450(4) 0.8577(4) 0.029(3) Uiso 0.453(11) 1 d PD B 1 F14A F 0.5525(10) 0.2545(10) 0.9255(6) 0.104(5) Uiso 0.453(11) 1 d PD B 1 F14B F 0.3635(11) 0.1235(4) 0.8055(5) 0.058(3) Uiso 0.453(11) 1 d PD B 1 F14C F 0.3119(12) 0.2869(7) 0.8887(7) 0.080(3) Uiso 0.453(11) 1 d PD B 1 C12' C 0.5162(7) 0.4496(4) 0.8299(3) 0.028(5) Uiso 0.547(11) 1 d PD B 2 F12Y F 0.6349(7) 0.4917(7) 0.9089(5) 0.0418(18) Uiso 0.547(11) 1 d PD B 2 F12Z F 0.3921(8) 0.4858(7) 0.8577(5) 0.0409(17) Uiso 0.547(11) 1 d PD B 2 C13' C 0.4687(7) 0.3080(4) 0.7897(2) 0.039(3) Uiso 0.547(11) 1 d PD B 2 F13Y F 0.5899(8) 0.2722(8) 0.7574(6) 0.072(3) Uiso 0.547(11) 1 d PD B 2 F13Z F 0.3438(8) 0.2642(7) 0.7138(4) 0.058(2) Uiso 0.547(11) 1 d PD B 2 C14' C 0.4095(5) 0.2462(3) 0.8559(3) 0.078(7) Uiso 0.547(11) 1 d PD B 2 F14X F 0.5079(8) 0.3043(6) 0.9431(3) 0.054(2) Uiso 0.547(11) 1 d PD B 2 F14Y F 0.4152(11) 0.1292(4) 0.8250(5) 0.089(4) Uiso 0.547(11) 1 d PD B 2 F14Z F 0.2550(6) 0.2398(8) 0.8532(6) 0.089(3) Uiso 0.547(11) 1 d PD B 2 N21 N 0.7397(5) 0.4778(3) 0.4951(3) 0.0252(7) Uani 1 1 d . . . C22 C 0.6963(5) 0.3539(4) 0.4655(3) 0.0255(8) Uani 1 1 d . . . C23 C 0.7372(5) 0.2841(4) 0.3857(3) 0.0256(8) Uani 1 1 d . . . N24 N 0.8205(4) 0.3398(3) 0.3372(3) 0.0246(7) Uani 1 1 d . . . C25 C 0.8641(5) 0.4629(4) 0.3668(3) 0.0243(8) Uani 1 1 d . . . C26 C 0.8228(5) 0.5322(4) 0.4466(3) 0.0250(8) Uani 1 1 d . . . C27 C 0.6034(6) 0.2960(5) 0.5214(4) 0.0341(10) Uani 1 1 d . . . H27A H 0.6667 0.2551 0.5500 0.051 Uiso 1 1 calc R . . H27B H 0.5032 0.2354 0.4794 0.051 Uiso 1 1 calc R . . H27C H 0.5796 0.3599 0.5713 0.051 Uiso 1 1 calc R . . C28 C 0.6925(6) 0.1464(4) 0.3491(4) 0.0338(10) Uani 1 1 d . . . H28A H 0.5844 0.1111 0.3078 0.051 Uiso 1 1 calc R . . H28B H 0.6957 0.1195 0.4023 0.051 Uiso 1 1 calc R . . H28C H 0.7683 0.1186 0.3132 0.051 Uiso 1 1 calc R . . C29 C 0.9535(6) 0.5217(5) 0.3106(4) 0.0329(10) Uani 1 1 d . . . H29A H 0.9878 0.4605 0.2648 0.049 Uiso 1 1 calc R . . H29B H 1.0474 0.5894 0.3531 0.049 Uiso 1 1 calc R . . H29C H 0.8837 0.5540 0.2769 0.049 Uiso 1 1 calc R . . C30 C 0.8632(7) 0.6696(4) 0.4786(3) 0.0339(10) Uani 1 1 d . . . H30A H 0.7970 0.6904 0.4337 0.051 Uiso 1 1 calc R . . H30B H 0.9764 0.7046 0.4819 0.051 Uiso 1 1 calc R . . H30C H 0.8427 0.7034 0.5413 0.051 Uiso 1 1 calc R . . N31 N 1.3679(4) 0.9155(3) 0.9308(2) 0.0218(7) Uani 1 1 d . . . C32 C 1.5112(5) 0.8955(4) 0.9365(3) 0.0216(8) Uani 1 1 d . . . C36 C 1.3556(5) 1.0191(4) 0.9942(3) 0.0213(8) Uani 1 1 d . . . C37 C 1.5218(6) 0.7787(4) 0.8664(3) 0.0293(9) Uani 1 1 d . . . H37A H 1.4155 0.7179 0.8407 0.044 Uiso 1 1 calc R . . H37B H 1.5946 0.7464 0.8977 0.044 Uiso 1 1 calc R . . H37C H 1.5623 0.7956 0.8148 0.044 Uiso 1 1 calc R . . C40 C 1.1938(5) 1.0375(5) 0.9868(4) 0.0332(10) Uani 1 1 d . . . H40A H 1.1135 0.9618 0.9414 0.050 Uiso 1 1 calc R . . H40B H 1.1932 1.1051 0.9653 0.050 Uiso 1 1 calc R . . H40C H 1.1687 1.0577 1.0489 0.050 Uiso 1 1 calc R . . O1S O 0.9680(4) 0.7257(3) 0.8958(3) 0.0364(8) Uani 1 1 d . . . H1SO H 0.8926 0.6645 0.8610 0.055 Uiso 1 1 d R . . C1S C 1.0255(9) 0.6985(7) 0.9752(4) 0.0531(16) Uani 1 1 d . . . H1S1 H 0.9352 0.6736 1.0026 0.080 Uiso 1 1 calc R . . H1S2 H 1.1044 0.7738 1.0241 0.080 Uiso 1 1 calc R . . C2S C 1.1021(9) 0.5979(9) 0.9488(6) 0.064(2) Uani 1 1 d . . . H2S1 H 1.0227 0.5219 0.9031 0.096 Uiso 1 1 calc R . . H2S2 H 1.1434 0.5844 1.0055 0.096 Uiso 1 1 calc R . . H2S3 H 1.1902 0.6215 0.9205 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02569(19) 0.0318(2) 0.02501(19) 0.00333(14) 0.00327(13) 0.00984(14) Ag2 0.0543(3) 0.0296(2) 0.0306(2) 0.01152(16) 0.01865(17) 0.01803(17) O1A 0.053(3) 0.077(3) 0.054(3) 0.027(2) 0.008(2) 0.043(2) O1B 0.039(2) 0.0291(17) 0.0395(19) 0.0084(15) 0.0110(16) 0.0117(15) C1 0.038(3) 0.040(3) 0.026(2) 0.016(2) 0.0112(19) 0.022(2) C2 0.037(3) 0.036(3) 0.034(3) 0.005(2) 0.001(2) 0.006(2) O11A 0.0322(18) 0.043(2) 0.0351(18) 0.0168(16) 0.0054(15) 0.0140(15) O11B 0.0271(17) 0.0403(19) 0.0351(18) 0.0127(16) 0.0060(14) 0.0022(14) C11 0.031(2) 0.0212(19) 0.026(2) 0.0054(17) 0.0066(17) 0.0085(17) N21 0.0269(18) 0.0244(18) 0.0217(17) 0.0065(14) 0.0035(14) 0.0081(15) C22 0.024(2) 0.025(2) 0.023(2) 0.0080(17) 0.0015(16) 0.0063(17) C23 0.0218(19) 0.023(2) 0.027(2) 0.0057(17) 0.0007(16) 0.0067(16) N24 0.0194(16) 0.0260(18) 0.0242(17) 0.0050(14) 0.0020(13) 0.0081(14) C25 0.0186(18) 0.028(2) 0.0229(19) 0.0082(17) 0.0006(15) 0.0046(16) C26 0.025(2) 0.024(2) 0.023(2) 0.0068(16) 0.0013(16) 0.0062(16) C27 0.040(3) 0.029(2) 0.033(2) 0.0108(19) 0.013(2) 0.006(2) C28 0.037(3) 0.024(2) 0.037(3) 0.0079(19) 0.010(2) 0.0081(19) C29 0.035(2) 0.033(2) 0.032(2) 0.011(2) 0.013(2) 0.010(2) C30 0.049(3) 0.023(2) 0.028(2) 0.0074(18) 0.012(2) 0.009(2) N31 0.0201(16) 0.0218(16) 0.0212(16) 0.0055(13) 0.0038(13) 0.0068(13) C32 0.0227(19) 0.0211(18) 0.0218(19) 0.0071(15) 0.0072(15) 0.0085(15) C36 0.0167(17) 0.026(2) 0.0244(19) 0.0101(16) 0.0065(15) 0.0100(15) C37 0.026(2) 0.029(2) 0.028(2) 0.0031(18) 0.0052(17) 0.0115(18) C40 0.020(2) 0.034(2) 0.038(3) 0.003(2) 0.0025(18) 0.0124(18) O1S 0.0285(17) 0.0360(19) 0.0362(19) 0.0069(15) 0.0064(14) 0.0051(14) C1S 0.058(4) 0.061(4) 0.030(3) 0.012(3) 0.015(3) 0.006(3) C2S 0.055(4) 0.100(6) 0.059(4) 0.050(4) 0.018(3) 0.033(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N24 2.306(4) 2_766 ? Ag1 N31 2.328(4) . ? Ag1 O1S 2.385(4) . ? Ag1 O1A 2.471(4) . ? Ag2 N21 2.258(4) . ? Ag2 O1B 2.310(4) . ? Ag2 O11B 2.508(4) . ? Ag2 O11A 2.550(4) . ? O1A C1 1.221(6) . ? O1B C1 1.237(6) . ? C1 C2 1.5400(10) . ? C2 F2Y 1.341(9) . ? C2 F2B 1.3497(10) . ? C2 F2A 1.3497(10) . ? C2 F2Z 1.382(8) . ? C2 C3 1.5396(10) . ? C2 C3' 1.5399(10) . ? C3 F3A 1.3494(10) . ? C3 F3B 1.3495(10) . ? C3 C4 1.5393(10) . ? C4 F4A 1.3490(10) . ? C4 F4B 1.3490(10) . ? C4 F4C 1.3492(10) . ? C3' F3Z 1.3498(10) . ? C3' F3Y 1.3499(10) . ? C3' C4' 1.5394(10) . ? C4' F4X 1.3493(10) . ? C4' F4Z 1.3493(10) . ? C4' F4Y 1.3494(10) . ? O11A C11 1.242(6) . ? O11B C11 1.254(6) . ? C11 C12 1.5408(10) . ? C11 C12' 1.5407(10) . ? C12 F12B 1.3498(10) . ? C12 F12A 1.3499(10) . ? C12 C13 1.5385(10) . ? C13 F13A 1.3488(10) . ? C13 F13B 1.3500(10) . ? C13 C14 1.5379(10) . ? C14 F14C 1.3493(10) . ? C14 F14A 1.3496(10) . ? C14 F14B 1.3503(10) . ? C12' F12Z 1.3499(10) . ? C12' F12Y 1.3499(10) . ? C12' C13' 1.5387(10) . ? C13' F13Y 1.3494(10) . ? C13' F13Z 1.3506(10) . ? C13' C14' 1.5362(10) . ? C14' F14X 1.3474(10) . ? C14' F14Z 1.3477(10) . ? C14' F14Y 1.3488(10) . ? N21 C22 1.350(6) . ? N21 C26 1.341(6) . ? C22 C23 1.394(6) . ? C22 C27 1.500(6) . ? C23 N24 1.350(6) . ? C23 C28 1.499(6) . ? N24 C25 1.341(6) . ? N24 Ag1 2.306(4) 2_766 ? C25 C26 1.393(6) . ? C25 C29 1.496(6) . ? C26 C30 1.500(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? N31 C36 1.347(5) . ? N31 C32 1.344(5) . ? C32 C36 1.392(6) 2_877 ? C32 C37 1.500(6) . ? C36 C32 1.392(6) 2_877 ? C36 C40 1.497(6) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? O1S C1S 1.429(8) . ? O1S H1SO 0.8263 . ? C1S C2S 1.498(11) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 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 N24 Ag1 N31 122.83(13) 2_766 . ? N24 Ag1 O1S 128.43(13) 2_766 . ? N31 Ag1 O1S 99.49(12) . . ? N24 Ag1 O1A 89.87(14) 2_766 . ? N31 Ag1 O1A 126.23(15) . . ? O1S Ag1 O1A 86.76(15) . . ? N21 Ag2 O1B 131.84(14) . . ? N21 Ag2 O11B 116.73(13) . . ? O1B Ag2 O11B 106.48(13) . . ? N21 Ag2 O11A 120.66(13) . . ? O1B Ag2 O11A 102.02(13) . . ? O11B Ag2 O11A 52.05(11) . . ? C1 O1A Ag1 156.0(4) . . ? C1 O1B Ag2 108.4(3) . . ? O1A C1 O1B 129.5(4) . . ? O1A C1 C2 115.9(5) . . ? O1B C1 C2 114.7(4) . . ? F2B C2 F2A 106.31(11) . . ? F2Y C2 F2Z 105.0(5) . . ? F2B C2 C3 83.3(4) . . ? F2A C2 C3 120.4(6) . . ? F2Y C2 C1 113.5(5) . . ? F2B C2 C1 113.6(4) . . ? F2A C2 C1 110.9(5) . . ? F2Z C2 C1 109.2(4) . . ? C3 C2 C1 118.2(3) . . ? F2Y C2 C3' 81.2(5) . . ? F2Z C2 C3' 128.9(5) . . ? C1 C2 C3' 114.2(4) . . ? F3A C3 F3B 106.35(11) . . ? F3A C3 C4 107.7(5) . . ? F3B C3 C4 105.9(5) . . ? F3A C3 C2 109.7(5) . . ? F3B C3 C2 111.6(5) . . ? C4 C3 C2 115.20(11) . . ? F4A C4 F4B 106.39(11) . . ? F4A C4 F4C 104.5(9) . . ? F4B C4 F4C 106.38(11) . . ? F4A C4 C3 115.1(6) . . ? F4B C4 C3 110.7(5) . . ? F4C C4 C3 113.1(7) . . ? F3Z C3' F3Y 106.31(11) . . ? F3Z C3' C4' 103.7(6) . . ? F3Y C3' C4' 101.9(6) . . ? F3Z C3' C2 111.4(6) . . ? F3Y C3' C2 117.1(8) . . ? C4' C3' C2 115.1(5) . . ? F4X C4' F4Z 106.3(9) . . ? F4X C4' F4Y 106.34(11) . . ? F4Z C4' F4Y 106.36(11) . . ? F4X C4' C3' 113.9(7) . . ? F4Z C4' C3' 110.8(6) . . ? F4Y C4' C3' 112.6(6) . . ? C11 O11A Ag2 90.4(2) . . ? C11 O11B Ag2 92.0(2) . . ? O11A C11 O11B 125.5(3) . . ? O11A C11 C12 115.1(4) . . ? O11B C11 C12 119.3(4) . . ? O11A C11 C12' 118.4(4) . . ? O11B C11 C12' 116.0(4) . . ? F12B C12 F12A 106.29(11) . . ? F12B C12 C13 109.5(5) . . ? F12A C12 C13 110.1(5) . . ? F12B C12 C11 110.2(5) . . ? F12A C12 C11 109.5(5) . . ? C13 C12 C11 111.1(3) . . ? F13A C13 F13B 106.36(11) . . ? F13A C13 C14 111.2(5) . . ? F13B C13 C14 103.6(5) . . ? F13A C13 C12 111.0(6) . . ? F13B C13 C12 108.5(6) . . ? C14 C13 C12 115.53(11) . . ? F14C C14 F14A 115.7(3) . . ? F14C C14 F14B 106.22(11) . . ? F14A C14 F14B 106.29(11) . . ? F14C C14 C13 109.59(11) . . ? F14A C14 C13 109.42(11) . . ? F14B C14 C13 109.45(11) . . ? F12Z C12' F12Y 106.28(11) . . ? F12Z C12' C13' 109.3(5) . . ? F12Y C12' C13' 107.8(5) . . ? F12Z C12' C11 110.3(5) . . ? F12Y C12' C11 111.2(5) . . ? C13' C12' C11 111.7(3) . . ? F13Y C13' F13Z 106.24(11) . . ? F13Y C13' C14' 112.4(5) . . ? F13Z C13' C14' 104.5(4) . . ? F13Y C13' C12' 109.1(5) . . ? F13Z C13' C12' 108.4(5) . . ? C14' C13' C12' 115.60(11) . . ? F14X C14' F14Z 114.4(3) . . ? F14X C14' F14Y 106.47(11) . . ? F14Z C14' F14Y 106.55(11) . . ? F14X C14' C13' 109.91(11) . . ? F14Z C14' C13' 109.67(11) . . ? F14Y C14' C13' 109.62(11) . . ? C22 N21 C26 118.9(4) . . ? C22 N21 Ag2 122.0(3) . . ? C26 N21 Ag2 119.1(3) . . ? N21 C22 C23 120.3(4) . . ? N21 C22 C27 117.5(4) . . ? C23 C22 C27 122.2(4) . . ? N24 C23 C22 120.3(4) . . ? N24 C23 C28 116.7(4) . . ? C22 C23 C28 123.0(4) . . ? C25 N24 C23 119.3(4) . . ? C25 N24 Ag1 121.3(3) . 2_766 ? C23 N24 Ag1 118.7(3) . 2_766 ? N24 C25 C26 120.2(4) . . ? N24 C25 C29 118.0(4) . . ? C26 C25 C29 121.7(4) . . ? N21 C26 C25 120.9(4) . . ? N21 C26 C30 117.7(4) . . ? C25 C26 C30 121.3(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 N31 C32 118.6(4) . . ? C36 N31 Ag1 121.0(3) . . ? C32 N31 Ag1 120.2(3) . . ? N31 C32 C36 120.6(4) . 2_877 ? N31 C32 C37 117.9(4) . . ? C36 C32 C37 121.6(4) 2_877 . ? N31 C36 C32 120.8(4) . 2_877 ? N31 C36 C40 117.2(4) . . ? C32 C36 C40 122.0(4) 2_877 . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1S O1S Ag1 118.6(3) . . ? C1S O1S H1SO 105.8 . . ? Ag1 O1S H1SO 110.1 . . ? O1S C1S C2S 112.1(5) . . ? O1S C1S H1S1 109.2 . . ? C2S C1S H1S1 109.2 . . ? O1S C1S H1S2 109.2 . . ? C2S C1S H1S2 109.2 . . ? H1S1 C1S H1S2 107.9 . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.295 _refine_diff_density_min -1.862 _refine_diff_density_rms 0.146 data_ilb918m _database_code_depnum_ccdc_archive 'CCDC 903739' #TrackingRef '1-MeOH_150K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Ag4 F28 N6 O10' _chemical_formula_weight 1752.32 _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.800(2) _cell_length_b 12.268(3) _cell_length_c 14.904(4) _cell_angle_alpha 109.781(4) _cell_angle_beta 96.709(4) _cell_angle_gamma 104.522(4) _cell_volume 1429.4(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2434 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 1.500 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7338 _exptl_absorpt_correction_T_max 0.8894 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16491 _diffrn_reflns_av_R_equivalents 0.1325 _diffrn_reflns_av_sigmaI/netI 0.1877 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6418 _reflns_number_gt 2954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6418 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1508 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1670 _refine_ls_wR_factor_gt 0.1386 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.63821(7) 0.27084(6) 0.32089(5) 0.0321(2) Uani 1 1 d . . . Ag2 Ag 0.79827(9) -0.10788(6) -0.13085(5) 0.0387(2) Uani 1 1 d . . . O11A O 0.7897(6) -0.0543(5) -0.2724(4) 0.0337(15) Uani 1 1 d . . . O11B O 1.0453(7) 0.0039(6) -0.1946(5) 0.0378(16) Uani 1 1 d . . . O1S O 0.4630(7) 0.2086(5) 0.4155(5) 0.0382(16) Uani 1 1 d . . . H1SO H 0.3570 0.1551 0.3841 0.046 Uiso 1 1 d R . . N21 N 0.6716(7) 0.1494(6) 0.1733(5) 0.0256(16) Uani 1 1 d . . . N24 N 0.7418(8) 0.0108(6) 0.0055(5) 0.0242(16) Uani 1 1 d . . . N31 N 0.8621(7) 0.4098(6) 0.4374(5) 0.0251(16) Uani 1 1 d . . . O1A O 0.4505(8) 0.3502(6) 0.2449(5) 0.0523(19) Uani 1 1 d . . . O1B O 0.8088(7) -0.3032(5) -0.1799(5) 0.0375(16) Uani 1 1 d . . . F1 F 0.1267(9) 0.5220(7) 0.1013(6) 0.096(2) Uani 1 1 d . . . F4C F 0.3270(10) 0.5869(6) 0.0341(6) 0.096(3) Uani 1 1 d . . . F4B F 0.2636(10) 0.4084(6) 0.0338(5) 0.091(2) Uani 1 1 d . . . F3B F 0.5294(8) 0.5582(7) 0.1598(7) 0.102(3) Uani 1 1 d . . . F3A F 0.3995(10) 0.6891(6) 0.2235(6) 0.104(3) Uani 1 1 d . . . F2B F 0.2099(7) 0.5325(5) 0.2844(5) 0.0645(18) Uani 1 1 d . . . F2A F 0.4655(8) 0.5793(5) 0.3341(5) 0.078(2) Uani 1 1 d . . . F14C F 1.0904(11) 0.3770(6) -0.3087(6) 0.111(3) Uani 1 1 d . . . F9B F 0.9311(10) 0.2277(7) -0.4248(6) 0.106(3) Uiso 1 1 d . . . F14A F 1.1744(9) 0.2386(7) -0.3970(6) 0.092(2) Uani 1 1 d . . . F13B F 1.1464(10) 0.2423(8) -0.2124(6) 0.106(3) Uiso 1 1 d . . . F13A F 0.8956(8) 0.2132(7) -0.2547(5) 0.091(2) Uiso 1 1 d . . . F12A F 0.8789(7) 0.0056(5) -0.4153(4) 0.0606(17) Uani 1 1 d . . . F14 F 1.1262(6) 0.0332(5) -0.3549(4) 0.0592(17) Uani 1 1 d . . . C4 C 0.2750(18) 0.5224(11) 0.0863(10) 0.072(4) Uani 1 1 d . . . C3 C 0.3827(16) 0.5681(9) 0.1802(9) 0.068(4) Uani 1 1 d . . . C2 C 0.3435(12) 0.5114(8) 0.2568(7) 0.042(2) Uani 1 1 d . . . C1 C 0.3267(11) 0.3746(8) 0.2240(7) 0.033(2) Uani 1 1 d . . . C14 C 1.0574(14) 0.2618(9) -0.3532(8) 0.054(3) Uani 1 1 d . . . C13 C 1.0219(12) 0.1924(11) -0.2884(10) 0.062(3) Uani 1 1 d . . . C12 C 0.9907(10) 0.0542(8) -0.3307(6) 0.030(2) Uani 1 1 d . . . C11 C 0.9395(11) -0.0049(8) -0.2592(7) 0.031(2) Uani 1 1 d . . . C22 C 0.7559(9) 0.2023(7) 0.1219(6) 0.028(2) Uani 1 1 d . . . C26 C 0.6260(9) 0.0287(7) 0.1449(6) 0.0250(19) Uani 1 1 d . . . C25 C 0.6587(9) -0.0418(7) 0.0592(6) 0.027(2) Uani 1 1 d . . . C23 C 0.7911(9) 0.1325(7) 0.0380(6) 0.027(2) Uani 1 1 d . . . C27 C 0.8062(10) 0.3385(7) 0.1573(6) 0.034(2) Uani 1 1 d . . . H13A H 0.7264 0.3684 0.1905 0.051 Uiso 1 1 calc R . . H13B H 0.8137 0.3631 0.1015 0.051 Uiso 1 1 calc R . . H13C H 0.9113 0.3731 0.2030 0.051 Uiso 1 1 calc R . . C30 C 0.5405(10) -0.0287(8) 0.2075(6) 0.034(2) Uani 1 1 d . . . H14A H 0.5293 0.0352 0.2649 0.051 Uiso 1 1 calc R . . H14B H 0.6032 -0.0747 0.2288 0.051 Uiso 1 1 calc R . . H14C H 0.4337 -0.0838 0.1694 0.051 Uiso 1 1 calc R . . C29 C 0.6104(10) -0.1786(7) 0.0250(7) 0.037(2) Uani 1 1 d . . . H15A H 0.6141 -0.2136 -0.0440 0.056 Uiso 1 1 calc R . . H15B H 0.5008 -0.2096 0.0328 0.056 Uiso 1 1 calc R . . H15C H 0.6848 -0.2015 0.0641 0.056 Uiso 1 1 calc R . . C28 C 0.8917(10) 0.1883(8) -0.0189(6) 0.036(2) Uani 1 1 d . . . H16A H 0.8994 0.1237 -0.0771 0.053 Uiso 1 1 calc R . . H16B H 0.9998 0.2357 0.0219 0.053 Uiso 1 1 calc R . . H16C H 0.8419 0.2420 -0.0388 0.053 Uiso 1 1 calc R . . C32 C 0.8553(9) 0.5171(7) 0.4986(6) 0.0239(19) Uani 1 1 d . . . C33 C 0.9933(9) 0.6095(7) 0.5609(6) 0.0216(18) Uani 1 1 d . . . C37 C 0.6899(8) 0.5341(8) 0.4947(7) 0.038(2) Uani 1 1 d . . . H19A H 0.6948 0.6117 0.4882 0.056 Uiso 1 1 calc R . . H19B H 0.6554 0.5344 0.5549 0.056 Uiso 1 1 calc R . . H19C H 0.6129 0.4671 0.4384 0.056 Uiso 1 1 calc R . . C38 C 0.9863(9) 0.7278(7) 0.6269(6) 0.032(2) Uani 1 1 d . . . H20A H 0.9755 0.7245 0.6908 0.048 Uiso 1 1 calc R . . H20B H 0.8935 0.7457 0.5990 0.048 Uiso 1 1 calc R . . H20C H 1.0853 0.7920 0.6350 0.048 Uiso 1 1 calc R . . C1S C 0.5162(12) 0.1621(10) 0.4851(8) 0.059(3) Uani 1 1 d . . . H21A H 0.5337 0.0842 0.4508 0.089 Uiso 1 1 calc R . . H21B H 0.4342 0.1499 0.5230 0.089 Uiso 1 1 calc R . . H21C H 0.6172 0.2204 0.5293 0.089 Uiso 1 1 calc R . . _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 0.0269(4) 0.0288(4) 0.0337(4) 0.0045(3) 0.0068(3) 0.0077(3) Ag2 0.0556(5) 0.0282(4) 0.0362(4) 0.0113(3) 0.0200(4) 0.0165(4) O11A 0.023(3) 0.044(4) 0.034(4) 0.017(3) 0.006(3) 0.006(3) O11B 0.027(3) 0.047(4) 0.038(4) 0.016(3) 0.006(3) 0.010(3) O1S 0.028(3) 0.035(4) 0.043(4) 0.012(3) 0.005(3) 0.000(3) N21 0.015(3) 0.031(4) 0.029(4) 0.007(3) 0.007(3) 0.009(3) N24 0.031(4) 0.025(4) 0.015(4) 0.005(3) 0.005(3) 0.010(3) N31 0.013(3) 0.037(4) 0.027(4) 0.009(3) 0.006(3) 0.013(3) O1A 0.058(4) 0.064(5) 0.051(4) 0.028(4) 0.007(4) 0.039(4) O1B 0.038(4) 0.028(3) 0.046(4) 0.013(3) 0.010(3) 0.012(3) F1 0.073(5) 0.103(6) 0.110(7) 0.033(5) 0.023(5) 0.035(4) F4C 0.150(7) 0.059(4) 0.100(6) 0.065(5) 0.030(5) 0.016(4) F4B 0.156(7) 0.051(4) 0.070(5) 0.027(4) 0.039(5) 0.027(4) F3B 0.048(4) 0.125(7) 0.161(8) 0.078(6) 0.042(5) 0.038(4) F3A 0.164(8) 0.029(4) 0.100(6) 0.027(4) 0.000(6) 0.010(4) F2B 0.072(4) 0.042(3) 0.084(5) 0.015(3) 0.031(4) 0.031(3) F2A 0.078(5) 0.049(4) 0.067(5) -0.001(3) -0.026(4) 0.004(3) F14C 0.206(9) 0.031(4) 0.110(6) 0.033(4) 0.070(6) 0.037(5) F14A 0.101(5) 0.088(5) 0.132(7) 0.068(5) 0.078(5) 0.043(5) F12A 0.061(4) 0.067(4) 0.043(4) 0.029(3) 0.002(3) -0.004(3) F14 0.053(4) 0.063(4) 0.081(4) 0.035(4) 0.043(3) 0.029(3) C4 0.105(11) 0.048(8) 0.074(10) 0.031(7) 0.034(9) 0.025(8) C3 0.100(10) 0.022(6) 0.073(9) 0.028(6) -0.005(8) 0.002(6) C2 0.050(6) 0.030(5) 0.039(6) 0.008(5) 0.001(5) 0.013(5) C1 0.039(6) 0.029(5) 0.034(5) 0.010(4) 0.007(5) 0.016(5) C14 0.074(8) 0.036(6) 0.044(7) 0.015(5) 0.008(6) 0.004(6) C13 0.034(6) 0.072(8) 0.111(10) 0.065(8) 0.024(7) 0.026(6) C12 0.024(5) 0.033(5) 0.032(5) 0.015(4) 0.006(4) 0.002(4) C11 0.036(5) 0.024(5) 0.031(5) 0.002(4) 0.014(5) 0.014(4) C22 0.020(4) 0.029(5) 0.029(5) 0.004(4) 0.001(4) 0.008(4) C26 0.022(4) 0.027(5) 0.028(5) 0.010(4) 0.002(4) 0.014(4) C25 0.023(4) 0.028(5) 0.031(5) 0.015(4) 0.003(4) 0.009(4) C23 0.020(4) 0.026(5) 0.035(5) 0.012(4) 0.001(4) 0.008(4) C27 0.038(5) 0.020(5) 0.038(5) 0.005(4) 0.006(4) 0.008(4) C30 0.025(5) 0.031(5) 0.043(6) 0.011(4) 0.008(4) 0.007(4) C29 0.035(5) 0.028(5) 0.044(6) 0.006(4) 0.015(5) 0.009(4) C28 0.042(5) 0.032(5) 0.030(5) 0.009(4) 0.017(4) 0.007(4) C32 0.021(4) 0.029(5) 0.026(5) 0.012(4) 0.005(4) 0.011(4) C33 0.017(4) 0.018(4) 0.025(5) 0.002(4) 0.007(3) 0.007(3) C37 0.011(4) 0.045(6) 0.048(6) 0.006(5) 0.002(4) 0.013(4) C38 0.021(4) 0.033(5) 0.030(5) -0.003(4) -0.003(4) 0.012(4) C1S 0.044(6) 0.057(7) 0.060(8) 0.012(6) -0.001(6) 0.007(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. ; _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 N21 2.302(6) . ? Ag1 N31 2.306(6) . ? Ag1 O1S 2.365(6) . ? Ag1 O1A 2.465(6) . ? Ag2 N24 2.257(6) . ? Ag2 O1B 2.286(6) . ? Ag2 O11A 2.411(6) . ? O11A C11 1.266(10) . ? O11B C11 1.214(10) . ? O1S C1S 1.429(12) . ? O1S H1SO 0.9499 . ? N21 C26 1.331(10) . ? N21 C22 1.337(10) . ? N24 C23 1.337(10) . ? N24 C25 1.356(10) . ? N31 C32 1.344(9) . ? N31 C33 1.351(9) 2_766 ? O1A C1 1.233(10) . ? O1B C1 1.234(10) 2_655 ? F1 C4 1.348(14) . ? F4C C4 1.326(13) . ? F4B C4 1.323(12) . ? F3B C3 1.386(14) . ? F3A C3 1.365(11) . ? F2B C2 1.346(10) . ? F2A C2 1.337(10) . ? F14C C14 1.280(11) . ? F9B C14 1.318(12) . ? F14A C14 1.320(12) . ? F13B C13 1.327(13) . ? F13A C13 1.319(11) . ? F12A C12 1.349(9) . ? F14 C12 1.345(9) . ? C4 C3 1.436(17) . ? C3 C2 1.554(15) . ? C2 C1 1.544(12) . ? C1 O1B 1.234(10) 2_655 ? C14 C13 1.500(15) . ? C13 C12 1.532(13) . ? C12 C11 1.528(12) . ? C22 C23 1.375(11) . ? C22 C27 1.498(11) . ? C26 C25 1.388(11) . ? C26 C30 1.508(11) . ? C25 C29 1.506(11) . ? C23 C28 1.496(11) . ? C27 H13A 0.9800 . ? C27 H13B 0.9800 . ? C27 H13C 0.9800 . ? C30 H14A 0.9800 . ? C30 H14B 0.9800 . ? C30 H14C 0.9800 . ? C29 H15A 0.9800 . ? C29 H15B 0.9800 . ? C29 H15C 0.9800 . ? C28 H16A 0.9800 . ? C28 H16B 0.9800 . ? C28 H16C 0.9800 . ? C32 C33 1.398(10) . ? C32 C37 1.518(10) . ? C33 N31 1.351(9) 2_766 ? C33 C38 1.474(10) . ? C37 H19A 0.9800 . ? C37 H19B 0.9800 . ? C37 H19C 0.9800 . ? C38 H20A 0.9800 . ? C38 H20B 0.9800 . ? C38 H20C 0.9800 . ? C1S H21A 0.9800 . ? C1S H21B 0.9800 . ? C1S H21C 0.9800 . ? _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 N21 Ag1 N31 119.1(2) . . ? N21 Ag1 O1S 126.5(2) . . ? N31 Ag1 O1S 103.1(2) . . ? N21 Ag1 O1A 93.7(2) . . ? N31 Ag1 O1A 117.9(2) . . ? O1S Ag1 O1A 94.1(2) . . ? N24 Ag2 O1B 131.3(2) . . ? N24 Ag2 O11A 119.7(2) . . ? O1B Ag2 O11A 107.2(2) . . ? C11 O11A Ag2 97.4(5) . . ? C1S O1S Ag1 120.1(5) . . ? C1S O1S H1SO 103.9 . . ? Ag1 O1S H1SO 119.6 . . ? C26 N21 C22 119.8(7) . . ? C26 N21 Ag1 120.9(5) . . ? C22 N21 Ag1 118.7(5) . . ? C23 N24 C25 117.8(7) . . ? C23 N24 Ag2 122.7(5) . . ? C25 N24 Ag2 119.5(5) . . ? C32 N31 C33 118.3(6) . 2_766 ? C32 N31 Ag1 120.8(5) . . ? C33 N31 Ag1 120.5(5) 2_766 . ? C1 O1A Ag1 159.5(7) . . ? C1 O1B Ag2 109.2(5) 2_655 . ? F4C C4 F4B 106.2(10) . . ? F4C C4 F1 113.3(12) . . ? F4B C4 F1 106.5(11) . . ? F4C C4 C3 110.9(11) . . ? F4B C4 C3 112.0(11) . . ? F1 C4 C3 107.8(11) . . ? F3A C3 F3B 107.7(9) . . ? F3A C3 C4 107.3(10) . . ? F3B C3 C4 105.0(11) . . ? F3A C3 C2 106.6(10) . . ? F3B C3 C2 109.0(9) . . ? C4 C3 C2 120.6(10) . . ? F2A C2 F2B 106.4(8) . . ? F2A C2 C3 103.3(8) . . ? F2B C2 C3 109.0(9) . . ? F2A C2 C1 111.7(8) . . ? F2B C2 C1 110.6(8) . . ? C3 C2 C1 115.3(8) . . ? O1A C1 O1B 128.1(8) . 2_655 ? O1A C1 C2 115.9(8) . . ? O1B C1 C2 116.0(8) 2_655 . ? F14C C14 F14A 109.5(10) . . ? F14C C14 F9B 106.2(10) . . ? F14A C14 F9B 105.0(9) . . ? F14C C14 C13 113.3(10) . . ? F14A C14 C13 112.2(10) . . ? F9B C14 C13 110.1(10) . . ? F13A C13 F13B 106.9(11) . . ? F13A C13 C14 107.7(9) . . ? F13B C13 C14 106.2(9) . . ? F13A C13 C12 107.9(8) . . ? F13B C13 C12 108.5(8) . . ? C14 C13 C12 118.9(10) . . ? F14 C12 F12A 105.9(7) . . ? F14 C12 C11 110.2(7) . . ? F12A C12 C11 111.4(7) . . ? F14 C12 C13 108.1(7) . . ? F12A C12 C13 108.4(8) . . ? C11 C12 C13 112.6(8) . . ? O11B C11 O11A 127.3(9) . . ? O11B C11 C12 116.9(8) . . ? O11A C11 C12 115.7(8) . . ? N21 C22 C23 120.3(8) . . ? N21 C22 C27 117.9(7) . . ? C23 C22 C27 121.8(8) . . ? N21 C26 C25 119.7(8) . . ? N21 C26 C30 119.0(7) . . ? C25 C26 C30 121.3(7) . . ? N24 C25 C26 120.9(7) . . ? N24 C25 C29 117.7(7) . . ? C26 C25 C29 121.3(8) . . ? N24 C23 C22 121.3(8) . . ? N24 C23 C28 116.7(7) . . ? C22 C23 C28 121.9(8) . . ? C22 C27 H13A 109.5 . . ? C22 C27 H13B 109.5 . . ? H13A C27 H13B 109.5 . . ? C22 C27 H13C 109.5 . . ? H13A C27 H13C 109.5 . . ? H13B C27 H13C 109.5 . . ? C26 C30 H14A 109.5 . . ? C26 C30 H14B 109.5 . . ? H14A C30 H14B 109.5 . . ? C26 C30 H14C 109.5 . . ? H14A C30 H14C 109.5 . . ? H14B C30 H14C 109.5 . . ? C25 C29 H15A 109.5 . . ? C25 C29 H15B 109.5 . . ? H15A C29 H15B 109.5 . . ? C25 C29 H15C 109.5 . . ? H15A C29 H15C 109.5 . . ? H15B C29 H15C 109.5 . . ? C23 C28 H16A 109.5 . . ? C23 C28 H16B 109.5 . . ? H16A C28 H16B 109.5 . . ? C23 C28 H16C 109.5 . . ? H16A C28 H16C 109.5 . . ? H16B C28 H16C 109.5 . . ? N31 C32 C33 122.0(6) . . ? N31 C32 C37 116.4(7) . . ? C33 C32 C37 121.6(7) . . ? N31 C33 C32 119.7(6) 2_766 . ? N31 C33 C38 118.3(7) 2_766 . ? C32 C33 C38 122.1(6) . . ? C32 C37 H19A 109.5 . . ? C32 C37 H19B 109.5 . . ? H19A C37 H19B 109.5 . . ? C32 C37 H19C 109.5 . . ? H19A C37 H19C 109.5 . . ? H19B C37 H19C 109.5 . . ? C33 C38 H20A 109.5 . . ? C33 C38 H20B 109.5 . . ? H20A C38 H20B 109.5 . . ? C33 C38 H20C 109.5 . . ? H20A C38 H20C 109.5 . . ? H20B C38 H20C 109.5 . . ? O1S C1S H21A 109.5 . . ? O1S C1S H21B 109.5 . . ? H21A C1S H21B 109.5 . . ? O1S C1S H21C 109.5 . . ? H21A C1S H21C 109.5 . . ? H21B C1S H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.615 _refine_diff_density_min -1.365 _refine_diff_density_rms 0.169 data_ilb927s _database_code_depnum_ccdc_archive 'CCDC 903740' #TrackingRef '1-iPrOH_150K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Ag4 F28 N6 O10' _chemical_formula_weight 1812.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8970 1.1020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9624(6) _cell_length_b 12.0249(9) _cell_length_c 15.3602(16) _cell_angle_alpha 108.091(5) _cell_angle_beta 96.976(5) _cell_angle_gamma 103.206(4) _cell_volume 1498.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20779 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 36.69 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 1.434 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6982 _exptl_absorpt_correction_T_max 0.8468 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart 4000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 51533 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 37.13 _reflns_number_total 13972 _reflns_number_gt 10964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+1.8825P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13972 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.341644(18) 0.212889(15) 0.183806(11) 0.02204(4) Uani 1 1 d . . . Ag2 Ag 0.17761(2) 0.589390(16) 0.616757(13) 0.02890(5) Uani 1 1 d . . . O1 O -0.0458(2) 0.49387(19) 0.68226(14) 0.0322(4) Uani 1 1 d . . . O2 O 0.1960(2) 0.54466(18) 0.76594(13) 0.0300(4) Uani 1 1 d . . . O3 O 0.1802(2) 0.79464(16) 0.66418(13) 0.0265(3) Uani 1 1 d . . . O4 O 0.53822(19) 0.29397(16) 0.10863(12) 0.0243(3) Uani 1 1 d . . . H4 H 0.6335 0.3439 0.1511 0.029 Uiso 1 1 d R . . O5 O 0.5754(2) 0.1983(2) 0.27851(15) 0.0376(5) Uani 1 1 d . . . N1 N 0.2464(2) 0.47319(17) 0.49057(13) 0.0215(3) Uani 1 1 d . . . N2 N 0.3135(2) 0.33406(17) 0.32840(13) 0.0203(3) Uani 1 1 d . . . N3 N 0.12906(19) 0.08230(15) 0.06645(12) 0.0162(3) Uani 1 1 d . . . C1 C 0.0519(3) 0.4976(2) 0.74754(16) 0.0232(4) Uani 1 1 d . . . C2 C -0.0104(3) 0.4303(2) 0.81314(17) 0.0268(4) Uani 1 1 d . . . C3 C 0.0153(3) 0.3030(2) 0.78835(17) 0.0270(4) Uani 1 1 d . . . C4 C -0.0596(3) 0.2221(2) 0.84211(19) 0.0308(5) Uani 1 1 d . . . C5 C 0.3321(2) 0.5265(2) 0.44139(15) 0.0217(4) Uani 1 1 d . . . C6 C 0.3670(2) 0.4559(2) 0.35881(15) 0.0209(4) Uani 1 1 d . . . C7 C 0.2300(2) 0.2802(2) 0.37868(15) 0.0207(4) Uani 1 1 d . . . C8 C 0.1953(2) 0.3506(2) 0.46089(15) 0.0210(4) Uani 1 1 d . . . C9 C 0.3834(3) 0.6628(2) 0.47401(18) 0.0296(5) Uani 1 1 d . . . H9A H 0.3174 0.6908 0.4346 0.044 Uiso 1 1 calc R . . H9B H 0.4929 0.6905 0.4695 0.044 Uiso 1 1 calc R . . H9C H 0.3736 0.6963 0.5392 0.044 Uiso 1 1 calc R . . C10 C 0.4615(3) 0.5138(2) 0.30237(18) 0.0282(4) Uani 1 1 d . . . H10A H 0.4833 0.4504 0.2518 0.042 Uiso 1 1 calc R . . H10B H 0.5605 0.5699 0.3428 0.042 Uiso 1 1 calc R . . H10C H 0.4026 0.5590 0.2756 0.042 Uiso 1 1 calc R . . C11 C 0.1752(3) 0.1439(2) 0.34269(17) 0.0261(4) Uani 1 1 d . . . H11A H 0.0608 0.1167 0.3233 0.039 Uiso 1 1 calc R . . H11B H 0.2076 0.1137 0.3922 0.039 Uiso 1 1 calc R . . H11C H 0.2214 0.1118 0.2889 0.039 Uiso 1 1 calc R . . C12 C 0.1023(3) 0.2949(2) 0.51901(17) 0.0276(4) Uani 1 1 d . . . H12A H 0.1717 0.2732 0.5614 0.041 Uiso 1 1 calc R . . H12B H 0.0206 0.2214 0.4780 0.041 Uiso 1 1 calc R . . H12C H 0.0536 0.3536 0.5557 0.041 Uiso 1 1 calc R . . C13 C 0.5114(3) 0.3647(2) 0.05042(16) 0.0241(4) Uani 1 1 d . . . H13 H 0.5548 0.4484 0.0890 0.029 Uiso 1 1 d R . . C14 C 0.5877(4) 0.3307(3) -0.0331(2) 0.0387(6) Uani 1 1 d . . . H14A H 0.7010 0.3490 -0.0112 0.058 Uiso 1 1 calc R . . H14B H 0.5676 0.3777 -0.0729 0.058 Uiso 1 1 calc R . . H14C H 0.5440 0.2434 -0.0691 0.058 Uiso 1 1 calc R . . C15 C 0.3372(3) 0.3406(3) 0.0218(2) 0.0397(6) Uani 1 1 d . . . H15A H 0.2890 0.2532 -0.0121 0.059 Uiso 1 1 calc R . . H15B H 0.3156 0.3862 -0.0190 0.059 Uiso 1 1 calc R . . H15C H 0.2934 0.3669 0.0777 0.059 Uiso 1 1 calc R . . C16 C 0.6813(3) 0.1522(2) 0.29307(15) 0.0208(4) Uani 1 1 d . . . C17 C 0.6404(3) 0.0120(2) 0.25516(18) 0.0288(4) Uani 1 1 d . A . C18 C 0.5997(6) -0.0523(3) 0.3257(3) 0.0603(11) Uani 1 1 d . . . C19 C 0.7094(6) -0.0236(4) 0.4131(3) 0.0602(10) Uani 1 1 d . A . C20 C 0.1441(2) -0.01789(18) 0.00185(13) 0.0163(3) Uani 1 1 d . . . C21 C -0.0135(2) 0.10137(18) 0.06506(13) 0.0165(3) Uani 1 1 d . . . C22 C 0.3043(2) -0.0350(2) 0.00357(17) 0.0254(4) Uani 1 1 d . . . H22A H 0.3821 0.0402 0.0455 0.038 Uiso 1 1 calc R . . H22B H 0.3254 -0.0543 -0.0598 0.038 Uiso 1 1 calc R . . H22C H 0.3104 -0.1020 0.0261 0.038 Uiso 1 1 calc R . . C23 C -0.0272(3) 0.2151(2) 0.13596(16) 0.0235(4) Uani 1 1 d . . . H23A H -0.0694 0.1950 0.1869 0.035 Uiso 1 1 calc R . . H23B H -0.0975 0.2502 0.1059 0.035 Uiso 1 1 calc R . . H23C H 0.0766 0.2743 0.1614 0.035 Uiso 1 1 calc R . . F1 F 0.0632(3) 0.49489(17) 0.90304(12) 0.0474(5) Uani 1 1 d . . . F2 F -0.1648(2) 0.4164(2) 0.80940(17) 0.0525(5) Uani 1 1 d . . . F3 F 0.1700(2) 0.31491(18) 0.80510(15) 0.0410(4) Uani 1 1 d . . . F4 F -0.0428(3) 0.24082(17) 0.69682(12) 0.0469(5) Uani 1 1 d . . . F5 F -0.0256(2) 0.28160(16) 0.93263(12) 0.0358(3) Uani 1 1 d . . . F6 F -0.2136(2) 0.1845(2) 0.81394(16) 0.0528(5) Uani 1 1 d . . . F7 F -0.0050(3) 0.12538(18) 0.82641(17) 0.0539(6) Uani 1 1 d . . . F8 F 0.5071(2) -0.03622(19) 0.18882(16) 0.0545(5) Uani 1 1 d . . . F9 F 0.7523(3) -0.02542(17) 0.21417(17) 0.0532(6) Uani 1 1 d . . . F10A F 0.6207(10) -0.1813(6) 0.2752(4) 0.060(2) Uiso 0.426(11) 1 d P A 1 F10B F 0.5472(5) -0.1737(3) 0.2800(2) 0.0384(11) Uiso 0.574(11) 1 d P A 2 F11 F 0.4586(3) -0.0296(3) 0.3555(2) 0.0759(8) Uani 1 1 d . A . F12 F 0.8440(3) -0.0333(3) 0.3870(2) 0.0801(9) Uani 1 1 d . . . F13A F 0.7351(3) 0.0894(3) 0.4718(2) 0.0393(8) Uiso 0.682(7) 1 d P A 1 F13B F 0.6282(10) 0.0787(7) 0.4484(6) 0.060(2) Uiso 0.318(7) 1 d P A 2 F14 F 0.6481(3) -0.0998(2) 0.45689(18) 0.0663(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01795(7) 0.02365(8) 0.01890(7) 0.00176(5) 0.00067(5) 0.00473(5) Ag2 0.04131(11) 0.02280(8) 0.02316(8) 0.00506(6) 0.01063(7) 0.01223(7) O1 0.0254(8) 0.0400(10) 0.0317(9) 0.0133(8) 0.0009(7) 0.0118(7) O2 0.0215(7) 0.0338(9) 0.0294(8) 0.0096(7) 0.0012(6) 0.0022(7) O3 0.0225(7) 0.0240(8) 0.0289(8) 0.0043(6) 0.0023(6) 0.0073(6) O4 0.0203(7) 0.0278(8) 0.0230(7) 0.0091(6) 0.0011(5) 0.0046(6) O5 0.0330(9) 0.0411(11) 0.0358(10) 0.0061(8) -0.0046(8) 0.0215(9) N1 0.0226(8) 0.0212(8) 0.0171(7) 0.0025(6) 0.0012(6) 0.0066(6) N2 0.0167(7) 0.0217(8) 0.0189(7) 0.0024(6) 0.0009(6) 0.0065(6) N3 0.0130(6) 0.0174(7) 0.0168(7) 0.0045(5) 0.0020(5) 0.0042(5) C1 0.0228(9) 0.0234(9) 0.0220(9) 0.0045(7) 0.0049(7) 0.0088(7) C2 0.0268(10) 0.0289(11) 0.0250(10) 0.0060(8) 0.0095(8) 0.0106(8) C3 0.0273(10) 0.0263(10) 0.0248(10) 0.0048(8) 0.0090(8) 0.0066(8) C4 0.0287(11) 0.0289(11) 0.0322(12) 0.0092(9) 0.0089(9) 0.0042(9) C5 0.0206(8) 0.0213(9) 0.0180(8) 0.0014(7) 0.0002(7) 0.0054(7) C6 0.0163(7) 0.0230(9) 0.0188(8) 0.0027(7) 0.0001(6) 0.0052(7) C7 0.0184(8) 0.0208(9) 0.0197(8) 0.0030(7) 0.0006(6) 0.0067(7) C8 0.0201(8) 0.0223(9) 0.0175(8) 0.0031(7) 0.0006(6) 0.0068(7) C9 0.0371(12) 0.0209(10) 0.0243(10) 0.0019(8) 0.0070(9) 0.0039(9) C10 0.0250(10) 0.0271(11) 0.0279(11) 0.0049(9) 0.0083(8) 0.0039(8) C11 0.0292(10) 0.0204(9) 0.0256(10) 0.0033(8) 0.0062(8) 0.0072(8) C12 0.0308(11) 0.0267(11) 0.0227(10) 0.0055(8) 0.0073(8) 0.0069(9) C13 0.0241(9) 0.0225(9) 0.0223(9) 0.0066(8) 0.0015(7) 0.0033(8) C14 0.0555(18) 0.0354(14) 0.0267(12) 0.0095(10) 0.0144(12) 0.0146(13) C15 0.0234(11) 0.0418(15) 0.0537(17) 0.0273(14) -0.0059(11) 0.0015(10) C16 0.0222(8) 0.0234(9) 0.0174(8) 0.0065(7) 0.0036(7) 0.0083(7) C17 0.0297(11) 0.0260(11) 0.0268(11) 0.0074(9) 0.0022(9) 0.0051(9) C18 0.093(3) 0.0339(16) 0.0434(19) 0.0141(14) 0.0006(19) 0.0051(18) C19 0.076(3) 0.052(2) 0.061(2) 0.0302(19) 0.015(2) 0.020(2) C20 0.0127(7) 0.0177(8) 0.0177(8) 0.0041(6) 0.0032(6) 0.0056(6) C21 0.0141(7) 0.0173(8) 0.0165(7) 0.0037(6) 0.0033(6) 0.0044(6) C22 0.0153(8) 0.0285(10) 0.0288(10) 0.0026(8) 0.0035(7) 0.0102(7) C23 0.0211(9) 0.0212(9) 0.0226(9) -0.0008(7) 0.0038(7) 0.0078(7) F1 0.0830(15) 0.0304(8) 0.0214(7) 0.0027(6) 0.0134(8) 0.0095(9) F2 0.0350(9) 0.0716(14) 0.0785(15) 0.0439(12) 0.0349(10) 0.0308(10) F3 0.0299(8) 0.0467(10) 0.0638(12) 0.0316(9) 0.0248(8) 0.0188(7) F4 0.0740(14) 0.0319(9) 0.0236(8) 0.0009(6) 0.0126(8) 0.0048(9) F5 0.0382(9) 0.0393(9) 0.0298(8) 0.0139(7) 0.0087(6) 0.0074(7) F6 0.0293(9) 0.0628(13) 0.0535(12) 0.0239(10) 0.0011(8) -0.0124(9) F7 0.0750(15) 0.0330(9) 0.0680(14) 0.0233(9) 0.0396(12) 0.0218(10) F8 0.0416(10) 0.0391(10) 0.0561(13) -0.0004(9) -0.0140(9) -0.0026(8) F9 0.0517(11) 0.0283(9) 0.0728(14) -0.0003(9) 0.0267(11) 0.0161(8) F11 0.0419(12) 0.114(2) 0.0675(16) 0.0189(16) 0.0102(11) 0.0317(14) F12 0.0361(11) 0.0689(17) 0.117(2) 0.0107(16) 0.0199(14) 0.0075(11) F14 0.0897(19) 0.0573(14) 0.0571(14) 0.0407(12) 0.0095(13) 0.0049(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.3208(17) . ? Ag1 N2 2.3265(18) . ? Ag1 O4 2.4076(17) . ? Ag1 O5 2.4738(19) . ? Ag2 N1 2.2566(18) . ? Ag2 O3 2.3400(17) . ? Ag2 O2 2.506(2) . ? Ag2 O1 2.549(2) . ? O1 C1 1.230(3) . ? O2 C1 1.244(3) . ? O3 C16 1.249(3) 2_666 ? O4 C13 1.447(3) . ? O4 H4 0.9500 . ? O5 C16 1.235(3) . ? N1 C5 1.337(3) . ? N1 C8 1.347(3) . ? N2 C6 1.340(3) . ? N2 C7 1.344(3) . ? N3 C21 1.348(2) . ? N3 C20 1.348(2) . ? C1 C2 1.555(3) . ? C2 F2 1.347(3) . ? C2 F1 1.350(3) . ? C2 C3 1.537(3) . ? C3 F4 1.341(3) . ? C3 F3 1.345(3) . ? C3 C4 1.554(4) . ? C4 F5 1.311(3) . ? C4 F6 1.321(3) . ? C4 F7 1.328(3) . ? C5 C6 1.406(3) . ? C5 C9 1.496(3) . ? C6 C10 1.496(3) . ? C7 C8 1.400(3) . ? C7 C11 1.496(3) . ? C8 C12 1.496(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.504(4) . ? C13 C14 1.515(4) . ? C13 H13 0.9539 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O3 1.249(3) 2_666 ? C16 C17 1.540(3) . ? C17 F9 1.337(3) . ? C17 F8 1.350(3) . ? C17 C18 1.546(5) . ? C18 F10B 1.347(5) . ? C18 F11 1.451(6) . ? C18 C19 1.458(6) . ? C18 F10A 1.570(8) . ? C19 F13A 1.326(5) . ? C19 F12 1.335(5) . ? C19 F14 1.355(5) . ? C19 F13B 1.558(9) . ? C20 C21 1.401(3) 2 ? C20 C22 1.495(3) . ? C21 C20 1.401(3) 2 ? C21 C23 1.501(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 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 N3 Ag1 N2 122.62(6) . . ? N3 Ag1 O4 107.16(6) . . ? N2 Ag1 O4 119.74(6) . . ? N3 Ag1 O5 137.85(7) . . ? N2 Ag1 O5 83.18(7) . . ? O4 Ag1 O5 81.08(7) . . ? N1 Ag2 O3 130.56(7) . . ? N1 Ag2 O2 121.11(7) . . ? O3 Ag2 O2 103.82(7) . . ? N1 Ag2 O1 119.81(7) . . ? O3 Ag2 O1 103.10(6) . . ? O2 Ag2 O1 52.23(6) . . ? C1 O1 Ag2 88.83(15) . . ? C1 O2 Ag2 90.50(15) . . ? C16 O3 Ag2 102.29(14) 2_666 . ? C13 O4 Ag1 122.70(13) . . ? C13 O4 H4 102.8 . . ? Ag1 O4 H4 113.2 . . ? C16 O5 Ag1 154.28(17) . . ? C5 N1 C8 119.30(18) . . ? C5 N1 Ag2 119.65(14) . . ? C8 N1 Ag2 120.95(15) . . ? C6 N2 C7 119.46(18) . . ? C6 N2 Ag1 121.75(15) . . ? C7 N2 Ag1 118.55(14) . . ? C21 N3 C20 118.84(17) . . ? C21 N3 Ag1 120.51(13) . . ? C20 N3 Ag1 120.53(12) . . ? O1 C1 O2 128.2(2) . . ? O1 C1 C2 116.4(2) . . ? O2 C1 C2 115.4(2) . . ? F2 C2 F1 106.9(2) . . ? F2 C2 C3 107.6(2) . . ? F1 C2 C3 107.7(2) . . ? F2 C2 C1 111.8(2) . . ? F1 C2 C1 110.4(2) . . ? C3 C2 C1 112.19(18) . . ? F4 C3 F3 108.2(2) . . ? F4 C3 C2 109.1(2) . . ? F3 C3 C2 109.1(2) . . ? F4 C3 C4 107.0(2) . . ? F3 C3 C4 106.8(2) . . ? C2 C3 C4 116.3(2) . . ? F5 C4 F6 108.4(2) . . ? F5 C4 F7 107.9(2) . . ? F6 C4 F7 108.8(2) . . ? F5 C4 C3 111.5(2) . . ? F6 C4 C3 110.6(2) . . ? F7 C4 C3 109.6(2) . . ? N1 C5 C6 120.7(2) . . ? N1 C5 C9 118.39(19) . . ? C6 C5 C9 120.9(2) . . ? N2 C6 C5 120.0(2) . . ? N2 C6 C10 118.52(19) . . ? C5 C6 C10 121.5(2) . . ? N2 C7 C8 120.4(2) . . ? N2 C7 C11 117.48(19) . . ? C8 C7 C11 122.1(2) . . ? N1 C8 C7 120.1(2) . . ? N1 C8 C12 117.45(19) . . ? C7 C8 C12 122.4(2) . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C13 C15 107.8(2) . . ? O4 C13 C14 109.7(2) . . ? C15 C13 C14 112.3(2) . . ? O4 C13 H13 106.6 . . ? C15 C13 H13 108.3 . . ? C14 C13 H13 111.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 O3 128.0(2) . 2_666 ? O5 C16 C17 117.2(2) . . ? O3 C16 C17 114.80(19) 2_666 . ? F9 C17 F8 106.4(2) . . ? F9 C17 C16 111.0(2) . . ? F8 C17 C16 110.6(2) . . ? F9 C17 C18 110.4(3) . . ? F8 C17 C18 101.5(3) . . ? C16 C17 C18 116.2(2) . . ? F10B C18 F11 99.7(4) . . ? F10B C18 C19 110.9(4) . . ? F11 C18 C19 103.9(4) . . ? F10B C18 C17 109.3(3) . . ? F11 C18 C17 109.6(3) . . ? C19 C18 C17 121.2(4) . . ? F11 C18 F10A 125.4(4) . . ? C19 C18 F10A 96.7(4) . . ? C17 C18 F10A 101.2(4) . . ? F13A C19 F12 107.4(4) . . ? F13A C19 F14 107.2(4) . . ? F12 C19 F14 116.4(4) . . ? F13A C19 C18 113.6(4) . . ? F12 C19 C18 104.3(4) . . ? F14 C19 C18 108.2(4) . . ? F12 C19 F13B 137.7(5) . . ? F14 C19 F13B 100.0(4) . . ? C18 C19 F13B 82.4(4) . . ? N3 C20 C21 120.62(16) . 2 ? N3 C20 C22 117.65(17) . . ? C21 C20 C22 121.72(17) 2 . ? N3 C21 C20 120.53(17) . 2 ? N3 C21 C23 118.07(17) . . ? C20 C21 C23 121.39(17) 2 . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 O4 H4 O2 0.95 1.81 2.757(2) 172.5 2_666 _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.410 _refine_diff_density_min -1.687 _refine_diff_density_rms 0.123 data_ilb1295_0m _database_code_depnum_ccdc_archive 'CCDC 903741' #TrackingRef '2_150K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Ag4 F28 N4 O8' _chemical_formula_weight 1556.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.614(4) _cell_length_b 11.051(4) _cell_length_c 11.967(5) _cell_angle_alpha 71.73(2) _cell_angle_beta 71.83(2) _cell_angle_gamma 62.31(2) _cell_volume 1157.0(7) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 1840 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.833 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6279 _exptl_absorpt_correction_T_max 0.9303 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18039 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_sigmaI/netI 0.1123 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.64 _reflns_number_total 5261 _reflns_number_gt 3092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5261 _refine_ls_number_parameters 319 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1704 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.19739(7) 0.44199(7) 0.44349(6) 0.0281(2) Uani 1 1 d . . . Ag2 Ag 0.41225(7) 0.16099(7) 0.55927(6) 0.0289(2) Uani 1 1 d . . . N21 N 0.5499(7) 0.2635(7) 0.5702(6) 0.0253(16) Uani 1 1 d . . . N24 N 0.3030(7) 0.5833(7) 0.4333(6) 0.0238(15) Uani 1 1 d . . . C23 C 0.2431(9) 0.6818(9) 0.5022(7) 0.0253(18) Uani 1 1 d . . . C22 C 0.6809(9) 0.2433(9) 0.4985(7) 0.0269(19) Uani 1 1 d . . . C29 C 0.4908(9) 0.4659(9) 0.2773(7) 0.0286(19) Uani 1 1 d . . . H29A H 0.4458 0.3989 0.3119 0.043 Uiso 1 1 calc R . . H29B H 0.5963 0.4162 0.2704 0.043 Uiso 1 1 calc R . . H29C H 0.4683 0.5152 0.1976 0.043 Uiso 1 1 calc R . . C27 C 0.3523(9) 0.3632(9) 0.7295(7) 0.029(2) Uani 1 1 d . . . H27A H 0.2730 0.4146 0.6850 0.044 Uiso 1 1 calc R . . H27B H 0.3349 0.4119 0.7922 0.044 Uiso 1 1 calc R . . H27C H 0.3569 0.2690 0.7665 0.044 Uiso 1 1 calc R . . C25 C 0.4324(9) 0.5695(8) 0.3575(7) 0.0243(18) Uani 1 1 d . . . C28 C 0.0929(9) 0.7038(9) 0.5765(8) 0.034(2) Uani 1 1 d . . . H28A H 0.0206 0.7843 0.5343 0.051 Uiso 1 1 calc R . . H28B H 0.0851 0.7210 0.6544 0.051 Uiso 1 1 calc R . . H28C H 0.0756 0.6204 0.5889 0.051 Uiso 1 1 calc R . . C26 C 0.4939(9) 0.3543(8) 0.6448(7) 0.0242(18) Uani 1 1 d . . . C30 C 0.7471(10) 0.1333(10) 0.4226(8) 0.040(2) Uani 1 1 d . . . H30A H 0.6721 0.1068 0.4198 0.060 Uiso 1 1 calc R . . H30B H 0.8244 0.0510 0.4579 0.060 Uiso 1 1 calc R . . H30C H 0.7877 0.1708 0.3410 0.060 Uiso 1 1 calc R . . O11A O 0.1966(6) 0.1616(6) 0.6783(6) 0.0369(15) Uani 1 1 d . A . O11B O 0.0435(6) 0.3799(6) 0.6182(5) 0.0313(14) Uani 1 1 d . . . C11 C 0.0770(7) 0.2636(9) 0.6915(5) 0.0294(19) Uiso 1 1 d D . . C12 C -0.0385(6) 0.2550(9) 0.8062(4) 0.049(12) Uiso 0.606(14) 1 d PD A 1 C13 C -0.0142(6) 0.2996(8) 0.9046(5) 0.051(7) Uiso 0.606(14) 1 d PD A 1 F12A F -0.1724(8) 0.3513(9) 0.7906(8) 0.028(2) Uiso 0.606(14) 1 d PD A 1 F14A F -0.2628(5) 0.3882(10) 0.9952(7) 0.088(6) Uiso 0.606(14) 1 d PD A 1 F13A F -0.0211(10) 0.4305(8) 0.8609(8) 0.041(3) Uiso 0.606(14) 1 d PD A 1 F12B F -0.0414(11) 0.1295(8) 0.8237(12) 0.063(4) Uiso 0.606(14) 1 d PD A 1 F13B F 0.1185(8) 0.2204(10) 0.9323(9) 0.055(3) Uiso 0.606(14) 1 d PD A 1 F14B F -0.1272(10) 0.1797(7) 1.0737(6) 0.064(3) Uiso 0.606(14) 1 d PD A 1 F14C F -0.0959(9) 0.3480(11) 1.0996(6) 0.050(3) Uiso 0.606(14) 1 d PD A 1 C14 C -0.1296(5) 0.3078(6) 1.0213(4) 0.043(5) Uiso 0.606(14) 1 d PD A 1 F13Z F 0.0332(15) 0.3807(13) 0.8844(14) 0.053(5) Uiso 0.394(14) 1 d PD A 2 F12Z F -0.1663(11) 0.3071(14) 0.7815(13) 0.036(4) Uiso 0.394(14) 1 d PD A 2 F13Y F 0.1134(11) 0.1566(12) 0.9416(12) 0.039(4) Uiso 0.394(14) 1 d PD A 2 F12Y F -0.0093(13) 0.1101(10) 0.8570(12) 0.026(3) Uiso 0.394(14) 1 d PD A 2 F14Y F -0.1624(11) 0.1712(9) 1.0504(8) 0.049(4) Uiso 0.394(14) 1 d PD A 2 F14X F -0.0679(12) 0.2572(19) 1.1245(7) 0.078(6) Uiso 0.394(14) 1 d PD A 2 F14Z F -0.2430(9) 0.3959(9) 1.0134(9) 0.018(3) Uiso 0.394(14) 1 d PD A 2 C12' C -0.0327(9) 0.2449(11) 0.8080(5) 0.015(10) Uiso 0.394(14) 1 d PD A 2 C13' C -0.0053(6) 0.2724(11) 0.9148(7) 0.036(8) Uiso 0.394(14) 1 d PD A 2 C14' C -0.1231(7) 0.2773(9) 1.0295(5) 0.050(9) Uiso 0.394(14) 1 d PD A 2 O1A O 0.4269(6) 0.0959(6) 0.3854(5) 0.0335(14) Uani 1 1 d . . . O1B O 0.2331(6) 0.2922(6) 0.3308(5) 0.0345(15) Uani 1 1 d . B . C1 C 0.3309(9) 0.1722(9) 0.3233(6) 0.030(2) Uiso 1 1 d D . . C3 C 0.3571(11) 0.1877(12) 0.0990(7) 0.034(8) Uiso 0.42(2) 1 d PD B 1 C2 C 0.3364(10) 0.1028(9) 0.2276(6) 0.024(7) Uiso 0.42(2) 1 d PD B 1 C4 C 0.4957(13) 0.2152(11) 0.0578(8) 0.036(6) Uiso 0.42(2) 1 d PD B 1 F2A F 0.4399(12) -0.0274(10) 0.2233(12) 0.023(3) Uiso 0.42(2) 1 d PD B 1 F3A F 0.3591(18) 0.1235(13) 0.0190(12) 0.023(5) Uiso 0.42(2) 1 d PD B 1 F4A F 0.6170(14) 0.0971(14) 0.0712(15) 0.043(4) Uiso 0.42(2) 1 d PD B 1 F3B F 0.292(2) 0.3260(11) 0.0563(15) 0.051(5) Uiso 0.42(2) 1 d PD B 1 F2B F 0.2080(10) 0.0936(16) 0.2498(13) 0.030(4) Uiso 0.42(2) 1 d PD B 1 F4B F 0.4936(15) 0.2991(13) 0.1202(9) 0.030(4) Uiso 0.42(2) 1 d PD B 1 F4C F 0.520(2) 0.2759(17) -0.0592(7) 0.060(5) Uiso 0.42(2) 1 d PD B 1 C3' C 0.3767(7) 0.1925(10) 0.0936(6) 0.032(5) Uiso 0.58(2) 1 d PD B 2 C2' C 0.3202(8) 0.1237(9) 0.2204(6) 0.035(6) Uiso 0.58(2) 1 d PD B 2 C4' C 0.5318(9) 0.1825(9) 0.0724(7) 0.033(4) Uiso 0.58(2) 1 d PD B 2 F2Z F 0.3982(11) -0.0153(9) 0.2309(11) 0.039(3) Uiso 0.58(2) 1 d PD B 2 F4Z F 0.6310(10) 0.0514(11) 0.1014(10) 0.046(3) Uiso 0.58(2) 1 d PD B 2 F4Y F 0.5383(14) 0.2587(11) 0.1376(8) 0.051(3) Uiso 0.58(2) 1 d PD B 2 F3Y F 0.2579(12) 0.3139(10) 0.0844(12) 0.049(4) Uiso 0.58(2) 1 d PD B 2 F2Y F 0.1837(7) 0.1471(13) 0.2198(9) 0.034(3) Uiso 0.58(2) 1 d PD B 2 F3Z F 0.3866(13) 0.1269(11) 0.0112(11) 0.042(5) Uiso 0.58(2) 1 d PD B 2 F4X F 0.5748(16) 0.2350(14) -0.0438(7) 0.058(4) Uiso 0.58(2) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0261(4) 0.0276(4) 0.0348(4) -0.0075(3) -0.0027(3) -0.0158(3) Ag2 0.0268(4) 0.0279(4) 0.0379(4) -0.0118(3) -0.0044(3) -0.0141(3) N21 0.025(4) 0.026(4) 0.026(4) -0.005(3) 0.002(3) -0.016(3) N24 0.021(3) 0.024(4) 0.028(4) -0.007(3) -0.002(3) -0.011(3) C23 0.028(4) 0.025(5) 0.020(4) -0.005(4) 0.001(3) -0.011(4) C22 0.027(4) 0.033(5) 0.025(4) -0.009(4) 0.008(4) -0.021(4) C29 0.030(5) 0.030(5) 0.030(5) -0.011(4) -0.003(4) -0.015(4) C27 0.036(5) 0.030(5) 0.030(5) -0.011(4) 0.003(4) -0.023(4) C25 0.028(4) 0.027(5) 0.017(4) -0.005(4) -0.001(3) -0.013(4) C28 0.027(5) 0.030(5) 0.041(5) -0.012(4) 0.001(4) -0.011(4) C26 0.029(4) 0.022(5) 0.027(4) -0.009(4) -0.006(4) -0.012(4) C30 0.030(5) 0.053(7) 0.042(6) -0.021(5) 0.009(4) -0.025(5) O11A 0.024(3) 0.033(4) 0.050(4) -0.012(3) 0.002(3) -0.013(3) O11B 0.020(3) 0.038(4) 0.036(3) -0.004(3) -0.001(3) -0.017(3) O1A 0.039(4) 0.029(4) 0.035(3) -0.009(3) -0.011(3) -0.011(3) O1B 0.027(3) 0.033(4) 0.048(4) -0.022(3) -0.005(3) -0.009(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 N24 2.266(6) . ? Ag1 O1B 2.280(6) . ? Ag1 O11B 2.350(5) . ? Ag1 O11B 2.558(6) 2_566 ? Ag1 Ag2 3.0748(16) . ? Ag2 N21 2.277(6) . ? Ag2 O11A 2.286(6) . ? Ag2 O1A 2.346(6) . ? Ag2 O1A 2.537(6) 2_656 ? N21 C22 1.344(9) . ? N21 C26 1.353(10) . ? N24 C25 1.359(9) . ? N24 C23 1.365(10) . ? C23 C22 1.395(11) 2_666 ? C23 C28 1.510(11) . ? C22 C23 1.395(11) 2_666 ? C22 C30 1.516(11) . ? C29 C25 1.508(11) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C27 C26 1.507(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C25 C26 1.381(11) 2_666 ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C26 C25 1.381(11) 2_666 ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? O11A C11 1.251(9) . ? O11B C11 1.270(9) . ? O11B Ag1 2.558(6) 2_566 ? C11 C12 1.5405(12) . ? C11 C12' 1.5405(12) . ? C12 F12A 1.3500(12) . ? C12 F12B 1.3501(11) . ? C12 C13 1.5394(11) . ? C13 F13A 1.3499(11) . ? C13 F13B 1.3500(12) . ? C13 C14 1.5382(12) . ? F14A C14 1.3489(12) . ? F14B C14 1.3489(12) . ? F14C C14 1.3493(11) . ? F13Z C13' 1.3495(11) . ? F12Z C12' 1.3498(12) . ? F13Y C13' 1.3499(12) . ? F12Y C12' 1.3499(12) . ? F14Y C14' 1.3487(11) . ? F14X C14' 1.3494(11) . ? F14Z C14' 1.3489(12) . ? C12' C13' 1.5390(11) . ? C13' C14' 1.5378(12) . ? O1A C1 1.258(9) . ? O1A Ag2 2.537(6) 2_656 ? O1B C1 1.258(10) . ? C1 C2 1.5399(11) . ? C1 C2' 1.5405(11) . ? C3 F3A 1.3496(11) . ? C3 F3B 1.3498(12) . ? C3 C2 1.5397(12) . ? C3 C4 1.5398(12) . ? C2 F2A 1.3499(12) . ? C2 F2B 1.3500(11) . ? C4 F4B 1.3498(11) . ? C4 F4A 1.3498(12) . ? C4 F4C 1.3499(12) . ? C3' F3Z 1.3502(11) . ? C3' F3Y 1.3506(12) . ? C3' C4' 1.5404(12) . ? C3' C2' 1.5405(12) . ? C2' F2Y 1.3503(11) . ? C2' F2Z 1.3503(12) . ? C4' F4X 1.3496(11) . ? C4' F4Y 1.3499(11) . ? C4' F4Z 1.3501(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N24 Ag1 O1B 135.2(2) . . ? N24 Ag1 O11B 122.5(2) . . ? O1B Ag1 O11B 101.1(2) . . ? N24 Ag1 O11B 101.2(2) . 2_566 ? O1B Ag1 O11B 93.7(2) . 2_566 ? O11B Ag1 O11B 82.7(2) . 2_566 ? N24 Ag1 Ag2 100.17(17) . . ? O1B Ag1 Ag2 76.54(16) . . ? O11B Ag1 Ag2 79.00(15) . . ? O11B Ag1 Ag2 157.10(13) 2_566 . ? N21 Ag2 O11A 129.2(2) . . ? N21 Ag2 O1A 123.9(2) . . ? O11A Ag2 O1A 104.4(2) . . ? N21 Ag2 O1A 101.7(2) . 2_656 ? O11A Ag2 O1A 99.3(2) . 2_656 ? O1A Ag2 O1A 82.5(2) . 2_656 ? N21 Ag2 Ag1 91.44(18) . . ? O11A Ag2 Ag1 79.21(16) . . ? O1A Ag2 Ag1 82.19(15) . . ? O1A Ag2 Ag1 163.68(13) 2_656 . ? C22 N21 C26 119.4(7) . . ? C22 N21 Ag2 121.5(5) . . ? C26 N21 Ag2 119.0(5) . . ? C25 N24 C23 117.7(7) . . ? C25 N24 Ag1 119.6(5) . . ? C23 N24 Ag1 122.6(5) . . ? N24 C23 C22 120.4(7) . 2_666 ? N24 C23 C28 116.3(7) . . ? C22 C23 C28 123.3(7) 2_666 . ? N21 C22 C23 120.6(7) . 2_666 ? N21 C22 C30 118.7(7) . . ? C23 C22 C30 120.7(7) 2_666 . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N24 C25 C26 121.5(7) . 2_666 ? N24 C25 C29 116.2(7) . . ? C26 C25 C29 122.2(7) 2_666 . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N21 C26 C25 120.1(7) . 2_666 ? N21 C26 C27 116.5(7) . . ? C25 C26 C27 123.4(7) 2_666 . ? C22 C30 H30A 109.5 . . ? C22 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C22 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C11 O11A Ag2 128.1(5) . . ? C11 O11B Ag1 125.9(4) . . ? C11 O11B Ag1 132.1(4) . 2_566 ? Ag1 O11B Ag1 97.3(2) . 2_566 ? O11A C11 O11B 124.6(5) . . ? O11A C11 C12 119.8(7) . . ? O11B C11 C12 115.6(7) . . ? O11A C11 C12' 116.2(8) . . ? O11B C11 C12' 119.2(7) . . ? F12A C12 F12B 106.26(11) . . ? F12A C12 C13 102.0(6) . . ? F12B C12 C13 121.8(8) . . ? F12A C12 C11 111.7(7) . . ? F12B C12 C11 105.4(7) . . ? C13 C12 C11 109.7(5) . . ? F13A C13 F13B 106.27(11) . . ? F13A C13 C14 105.4(5) . . ? F13B C13 C14 108.8(6) . . ? F13A C13 C12 107.3(6) . . ? F13B C13 C12 113.0(6) . . ? C14 C13 C12 115.37(11) . . ? F14A C14 F14B 106.42(11) . . ? F14A C14 F14C 115.3(3) . . ? F14B C14 F14C 106.37(11) . . ? F14A C14 C13 109.55(11) . . ? F14B C14 C13 109.52(11) . . ? F14C C14 C13 109.48(11) . . ? F12Z C12' F12Y 106.29(11) . . ? F12Z C12' C13' 120.9(9) . . ? F12Y C12' C13' 95.1(9) . . ? F12Z C12' C11 108.2(8) . . ? F12Y C12' C11 113.3(9) . . ? C13' C12' C11 112.3(6) . . ? F13Z C13' F13Y 106.31(11) . . ? F13Z C13' C14' 112.8(8) . . ? F13Y C13' C14' 105.7(7) . . ? F13Z C13' C12' 113.1(9) . . ? F13Y C13' C12' 102.3(9) . . ? C14' C13' C12' 115.45(11) . . ? F14Y C14' F14Z 106.44(11) . . ? F14Y C14' F14X 106.39(11) . . ? F14Z C14' F14X 115.2(3) . . ? F14Y C14' C13' 109.57(11) . . ? F14Z C14' C13' 109.59(11) . . ? F14X C14' C13' 109.49(11) . . ? C1 O1A Ag2 118.9(4) . . ? C1 O1A Ag2 138.3(5) . 2_656 ? Ag2 O1A Ag2 97.5(2) . 2_656 ? C1 O1B Ag1 129.9(5) . . ? O1A C1 O1B 129.3(5) . . ? O1A C1 C2 113.0(7) . . ? O1B C1 C2 117.7(7) . . ? O1A C1 C2' 121.2(7) . . ? O1B C1 C2' 109.5(7) . . ? F3A C3 F3B 106.33(11) . . ? F3A C3 C2 110.7(9) . . ? F3B C3 C2 129.9(13) . . ? F3A C3 C4 107.3(11) . . ? F3B C3 C4 83.3(13) . . ? C2 C3 C4 115.21(11) . . ? F2A C2 F2B 106.28(11) . . ? F2A C2 C3 105.3(8) . . ? F2B C2 C3 107.0(8) . . ? F2A C2 C1 116.6(9) . . ? F2B C2 C1 107.9(8) . . ? C3 C2 C1 113.1(7) . . ? F4B C4 F4A 106.30(11) . . ? F4B C4 F4C 106.27(11) . . ? F4A C4 F4C 104.9(12) . . ? F4B C4 C3 112.2(9) . . ? F4A C4 C3 112.6(9) . . ? F4C C4 C3 113.9(9) . . ? F3Z C3' F3Y 106.22(11) . . ? F3Z C3' C4' 103.3(8) . . ? F3Y C3' C4' 124.1(12) . . ? F3Z C3' C2' 110.2(9) . . ? F3Y C3' C2' 97.5(9) . . ? C4' C3' C2' 115.08(11) . . ? F2Y C2' F2Z 106.22(11) . . ? F2Y C2' C3' 105.1(6) . . ? F2Z C2' C3' 106.9(7) . . ? F2Y C2' C1 113.8(7) . . ? F2Z C2' C1 109.6(8) . . ? C3' C2' C1 114.6(6) . . ? F4X C4' F4Y 106.31(11) . . ? F4X C4' F4Z 108.5(9) . . ? F4Y C4' F4Z 106.25(11) . . ? F4X C4' C3' 110.1(7) . . ? F4Y C4' C3' 111.5(8) . . ? F4Z C4' C3' 113.8(6) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.64 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.448 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.202 data_ilb1114_0m _database_code_depnum_ccdc_archive 'CCDC 903742' #TrackingRef 'SCSC1_step0(start)_1-MeOH_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Ag4 F28 N6 O10' _chemical_formula_weight 1756.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8395(2) _cell_length_b 12.3964(2) _cell_length_c 15.1351(3) _cell_angle_alpha 109.8050(10) _cell_angle_beta 97.0750(10) _cell_angle_gamma 104.2180(10) _cell_volume 1473.34(5) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 9876 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 28.22 _exptl_crystal_description 'block from a needle' _exptl_crystal_colour needle _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.979 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 1.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7035 _exptl_absorpt_correction_T_max 0.9178 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37881 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.88 _reflns_number_total 6994 _reflns_number_gt 5373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+1.7451P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6994 _refine_ls_number_parameters 395 _refine_ls_number_restraints 289 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.2197 _refine_ls_wR_factor_gt 0.2089 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.254 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.64363(5) 0.77549(4) 0.81632(3) 0.04896(19) Uani 1 1 d . . . Ag2 Ag 0.19061(8) 0.59872(5) 0.62796(4) 0.0618(2) Uani 1 1 d . . . O1A O -0.0362(6) 0.4972(5) 0.6985(4) 0.0607(11) Uani 1 1 d U A . O1B O 0.2168(5) 0.5515(4) 0.7730(3) 0.0558(10) Uani 1 1 d U A . C1 C 0.0690(8) 0.5042(6) 0.7604(4) 0.0543(11) Uani 1 1 d DU . . C2 C 0.0224(9) 0.4512(5) 0.8353(4) 0.0634(13) Uiso 0.536(6) 1 d PDU A 1 F2A F -0.1019(9) 0.4833(9) 0.8680(7) 0.071(2) Uiso 0.536(6) 1 d PDU A 1 F2B F 0.1389(8) 0.4826(9) 0.9142(6) 0.070(2) Uiso 0.536(6) 1 d PDU A 1 C3 C -0.0309(10) 0.3131(5) 0.7834(4) 0.0790(15) Uiso 0.536(6) 1 d PDU A 1 F3A F -0.1699(9) 0.2661(9) 0.7163(6) 0.093(3) Uiso 0.536(6) 1 d PDU A 1 F3B F 0.0793(10) 0.2738(9) 0.7385(7) 0.088(2) Uiso 0.536(6) 1 d PDU A 1 C4 C -0.0524(9) 0.2421(5) 0.8494(7) 0.0890(17) Uiso 0.536(6) 1 d PDU A 1 F4A F -0.1438(14) 0.2773(8) 0.9120(7) 0.099(3) Uiso 0.536(6) 1 d PDU A 1 F4B F -0.1231(12) 0.1230(6) 0.7986(6) 0.099(3) Uiso 0.536(6) 1 d PDU A 1 F4C F 0.0824(11) 0.2528(10) 0.9086(9) 0.112(3) Uiso 0.536(6) 1 d PDU A 1 C2' C 0.0148(11) 0.4494(6) 0.8330(5) 0.0634(13) Uiso 0.464(6) 1 d PDU A 2 F2Y F 0.1102(10) 0.5193(9) 0.9211(6) 0.069(2) Uiso 0.464(6) 1 d PDU A 2 F2Z F -0.1356(9) 0.4499(10) 0.8405(8) 0.071(2) Uiso 0.464(6) 1 d PDU A 2 C3' C 0.0147(11) 0.3174(7) 0.7983(6) 0.0791(15) Uiso 0.464(6) 1 d PDU A 2 F3Y F -0.0761(12) 0.2517(11) 0.7082(7) 0.098(3) Uiso 0.464(6) 1 d PDU A 2 F3Z F 0.1646(10) 0.3119(10) 0.7946(8) 0.086(3) Uiso 0.464(6) 1 d PDU A 2 C4' C -0.0442(10) 0.2499(6) 0.8623(8) 0.0893(17) Uiso 0.464(6) 1 d PDU A 2 F4X F 0.0538(15) 0.3062(10) 0.9510(8) 0.107(3) Uiso 0.464(6) 1 d PDU A 2 F4Y F -0.0363(15) 0.1362(7) 0.8289(9) 0.106(3) Uiso 0.464(6) 1 d PDU A 2 F4Z F -0.1983(13) 0.2408(11) 0.8663(11) 0.103(3) Uiso 0.464(6) 1 d PDU A 2 O11A O 0.1784(6) 0.7935(5) 0.6739(4) 0.0649(11) Uani 1 1 d U B . O11B O 0.4342(7) 0.8356(5) 0.7389(5) 0.0804(13) Uani 1 1 d U B . C11 C 0.3149(9) 0.8612(5) 0.7181(6) 0.0662(11) Uani 1 1 d DU . . C12 C 0.3262(8) 0.9956(4) 0.7537(4) 0.0758(14) Uiso 0.605(6) 1 d PDU B 1 F12A F 0.4329(9) 1.0637(8) 0.8384(6) 0.092(2) Uiso 0.605(6) 1 d PDU B 1 F12B F 0.1856(7) 1.0160(7) 0.7661(6) 0.079(2) Uiso 0.605(6) 1 d PDU B 1 C13 C 0.3894(7) 1.0629(6) 0.6904(5) 0.0897(16) Uiso 0.605(6) 1 d PDU B 1 F13A F 0.4226(11) 1.1838(7) 0.7259(7) 0.101(3) Uiso 0.605(6) 1 d PDU B 1 F13B F 0.5228(12) 1.0403(9) 0.6646(9) 0.119(3) Uiso 0.605(6) 1 d PDU B 1 C14 C 0.2800(9) 1.0220(6) 0.5902(4) 0.0967(18) Uiso 0.605(6) 1 d PDU B 1 F14A F 0.3255(15) 1.0885(7) 0.5380(7) 0.115(3) Uiso 0.605(6) 1 d PDU B 1 F14B F 0.2625(11) 0.9068(6) 0.5339(7) 0.092(2) Uiso 0.605(6) 1 d PDU B 1 F14C F 0.1309(12) 1.0288(9) 0.5945(9) 0.119(3) Uiso 0.605(6) 1 d PDU B 1 C12' C 0.3402(12) 0.9977(4) 0.7528(6) 0.0765(14) Uiso 0.395(6) 1 d PDU B 2 F12Z F 0.2332(12) 1.0253(11) 0.8062(9) 0.080(2) Uiso 0.395(6) 1 d PDU B 2 F12Y F 0.4864(10) 1.0664(11) 0.8095(9) 0.080(3) Uiso 0.395(6) 1 d PDU B 2 C13' C 0.3040(12) 1.0550(10) 0.6802(8) 0.0887(16) Uiso 0.395(6) 1 d PDU B 2 F13Y F 0.1464(13) 1.0115(11) 0.6376(12) 0.105(3) Uiso 0.395(6) 1 d PDU B 2 F13Z F 0.3383(15) 1.1758(9) 0.7222(10) 0.087(3) Uiso 0.395(6) 1 d PDU B 2 C14' C 0.4056(13) 1.0431(10) 0.6038(8) 0.0988(19) Uiso 0.395(6) 1 d PDU B 2 F14X F 0.3989(19) 1.1043(15) 0.5455(11) 0.113(3) Uiso 0.395(6) 1 d PDU B 2 F14Y F 0.5572(17) 1.0873(13) 0.6573(10) 0.126(3) Uiso 0.395(6) 1 d PDU B 2 F14Z F 0.3754(18) 0.9228(10) 0.5609(11) 0.102(3) Uiso 0.395(6) 1 d PDU B 2 N21 N 0.8658(5) 0.9135(4) 0.9352(3) 0.0348(8) Uani 1 1 d U . . C22 C 0.8570(6) 1.0190(5) 0.9952(4) 0.0377(10) Uani 1 1 d U . . C26 C 1.0095(6) 0.8938(5) 0.9397(4) 0.0353(9) Uani 1 1 d U . . C27 C 0.6943(7) 1.0359(6) 0.9883(5) 0.0570(16) Uani 1 1 d U . . H27A H 0.6228 0.9756 0.9288 0.086 Uiso 1 1 calc R . . H27B H 0.7024 1.1157 0.9890 0.086 Uiso 1 1 calc R . . H27C H 0.6524 1.0273 1.0427 0.086 Uiso 1 1 calc R . . C28 C 1.0155(7) 0.7749(5) 0.8727(4) 0.0482(13) Uani 1 1 d U . . H28A H 1.0790 0.7426 0.9078 0.072 Uiso 1 1 calc R . . H28B H 1.0638 0.7860 0.8209 0.072 Uiso 1 1 calc R . . H28C H 0.9077 0.7193 0.8458 0.072 Uiso 1 1 calc R . . N31 N 0.2515(5) 0.4837(4) 0.4940(3) 0.0407(9) Uani 1 1 d U . . C32 C 0.3289(6) 0.5343(5) 0.4411(4) 0.0400(9) Uani 1 1 d U . . C33 C 0.3645(6) 0.4648(5) 0.3567(4) 0.0399(9) Uani 1 1 d U . . N34 N 0.3247(5) 0.3452(4) 0.3297(3) 0.0385(8) Uani 1 1 d U . . C35 C 0.2472(6) 0.2929(5) 0.3824(4) 0.0403(9) Uani 1 1 d U . . C36 C 0.2085(7) 0.3615(5) 0.4655(4) 0.0422(10) Uani 1 1 d U . . C37 C 0.3689(8) 0.6686(5) 0.4730(5) 0.0514(13) Uani 1 1 d U . . H37A H 0.3638 0.7032 0.5401 0.077 Uiso 1 1 calc R . . H37B H 0.2925 0.6876 0.4336 0.077 Uiso 1 1 calc R . . H37C H 0.4760 0.7018 0.4660 0.077 Uiso 1 1 calc R . . C38 C 0.4451(8) 0.5205(6) 0.2949(5) 0.0511(13) Uani 1 1 d U . . H38A H 0.4766 0.4608 0.2468 0.077 Uiso 1 1 calc R . . H38B H 0.5394 0.5872 0.3346 0.077 Uiso 1 1 calc R . . H38C H 0.3718 0.5498 0.2630 0.077 Uiso 1 1 calc R . . C39 C 0.2038(8) 0.1583(5) 0.3479(5) 0.0492(13) Uani 1 1 d U . . H39A H 0.2419 0.1274 0.2898 0.074 Uiso 1 1 calc R . . H39B H 0.0883 0.1239 0.3341 0.074 Uiso 1 1 calc R . . H39C H 0.2530 0.1364 0.3974 0.074 Uiso 1 1 calc R . . C40 C 0.1177(8) 0.3072(6) 0.5247(5) 0.0546(14) Uani 1 1 d U . . H40A H 0.1019 0.3705 0.5782 0.082 Uiso 1 1 calc R . . H40B H 0.1777 0.2637 0.5494 0.082 Uiso 1 1 calc R . . H40C H 0.0144 0.2521 0.4851 0.082 Uiso 1 1 calc R . . O1S O 0.4718(6) 0.7102(5) 0.9098(4) 0.0676(13) Uani 1 1 d U . . H1SO H 0.3893 0.6645 0.8740 0.101 Uiso 1 1 d R . . C1S C 0.5287(12) 0.6743(10) 0.9850(7) 0.089(2) Uani 1 1 d U . . H1S1 H 0.5453 0.5965 0.9567 0.133 Uiso 1 1 calc R . . H1S2 H 0.4502 0.6686 1.0240 0.133 Uiso 1 1 calc R . . H1S3 H 0.6291 0.7335 1.0251 0.133 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0408(3) 0.0494(3) 0.0415(3) 0.0008(2) 0.00510(19) 0.01330(19) Ag2 0.0915(4) 0.0519(3) 0.0472(3) 0.0140(2) 0.0279(3) 0.0323(3) O1A 0.050(2) 0.071(3) 0.058(3) 0.021(2) 0.006(2) 0.021(2) O1B 0.0479(19) 0.063(2) 0.053(2) 0.0204(18) 0.0126(17) 0.0131(17) C1 0.0519(16) 0.0573(17) 0.0562(17) 0.0206(15) 0.0159(15) 0.0209(15) O11A 0.065(2) 0.062(2) 0.069(2) 0.0194(19) 0.0153(19) 0.0307(19) O11B 0.074(2) 0.084(3) 0.086(3) 0.026(2) 0.004(2) 0.045(2) C11 0.0678(17) 0.0700(18) 0.0706(18) 0.0294(16) 0.0151(16) 0.0345(15) N21 0.0291(15) 0.0370(17) 0.0338(17) 0.0056(14) 0.0091(13) 0.0129(13) C22 0.0297(18) 0.040(2) 0.038(2) 0.0052(17) 0.0073(16) 0.0153(16) C26 0.0328(18) 0.0371(19) 0.0320(19) 0.0054(16) 0.0079(16) 0.0144(16) C27 0.030(2) 0.062(3) 0.058(3) -0.004(3) 0.000(2) 0.020(2) C28 0.045(3) 0.043(3) 0.045(3) -0.002(2) 0.006(2) 0.020(2) N31 0.0411(17) 0.0390(17) 0.0356(17) 0.0061(14) 0.0040(15) 0.0155(15) C32 0.0397(18) 0.0370(18) 0.0370(18) 0.0069(15) 0.0047(16) 0.0131(15) C33 0.0365(17) 0.0376(17) 0.0390(18) 0.0071(15) 0.0045(15) 0.0129(15) N34 0.0339(16) 0.0371(17) 0.0380(18) 0.0049(14) 0.0050(14) 0.0147(14) C35 0.0373(18) 0.0378(18) 0.0387(19) 0.0059(16) 0.0031(15) 0.0143(15) C36 0.0415(19) 0.0393(18) 0.0379(19) 0.0069(16) 0.0029(16) 0.0131(16) C37 0.067(3) 0.037(3) 0.042(3) 0.007(2) 0.011(3) 0.013(2) C38 0.053(3) 0.047(3) 0.047(3) 0.008(2) 0.018(2) 0.015(2) C39 0.050(3) 0.040(3) 0.049(3) 0.006(2) 0.011(2) 0.012(2) C40 0.060(3) 0.050(3) 0.045(3) 0.011(2) 0.012(3) 0.012(3) O1S 0.053(3) 0.083(3) 0.052(3) 0.020(2) 0.009(2) 0.007(2) C1S 0.082(4) 0.102(5) 0.061(4) 0.024(4) 0.004(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N34 2.307(4) 2_666 ? Ag1 N21 2.327(4) . ? Ag1 O1S 2.380(5) . ? Ag1 O11B 2.469(5) . ? Ag2 N31 2.263(4) . ? Ag2 O11A 2.310(5) . ? Ag2 O1B 2.454(5) . ? O1A C1 1.200(8) . ? O1B C1 1.254(8) . ? C1 C2' 1.5396(11) . ? C1 C2 1.5405(11) . ? C2 F2B 1.3501(11) . ? C2 F2A 1.3501(11) . ? C2 C3 1.5393(11) . ? C3 F3A 1.3493(11) . ? C3 F3B 1.3495(11) . ? C3 C4 1.5391(11) . ? C4 F4A 1.3496(11) . ? C4 F4C 1.3497(11) . ? C4 F4B 1.3500(11) . ? C2' F2Y 1.3500(11) . ? C2' F2Z 1.3499(11) . ? C2' C3' 1.5400(11) . ? C3' F3Z 1.3500(11) . ? C3' F3Y 1.3501(11) . ? C3' C4' 1.5398(11) . ? C4' F4Y 1.3492(11) . ? C4' F4Z 1.3495(11) . ? C4' F4X 1.3495(11) . ? O11A C11 1.237(9) . ? O11B C11 1.209(8) . ? C11 C12' 1.5398(11) . ? C11 C12 1.5401(11) . ? C12 F12B 1.3501(11) . ? C12 F12A 1.3503(11) . ? C12 C13 1.5396(11) . ? C13 F13B 1.3495(11) . ? C13 F13A 1.3497(11) . ? C13 C14 1.5394(11) . ? C14 F14B 1.3494(11) . ? C14 F14C 1.3495(11) . ? C14 F14A 1.3499(11) . ? C12' F12Y 1.3499(11) . ? C12' F12Z 1.3499(11) . ? C12' C13' 1.5397(11) . ? C13' F13Y 1.3497(11) . ? C13' F13Z 1.3500(11) . ? C13' C14' 1.5396(11) . ? C14' F14Z 1.3495(11) . ? C14' F14Y 1.3496(11) . ? C14' F14X 1.3496(11) . ? N21 C26 1.349(6) . ? N21 C22 1.343(6) . ? C22 C26 1.378(7) 2_777 ? C22 C27 1.499(7) . ? C26 C22 1.378(7) 2_777 ? C26 C28 1.497(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? N31 C32 1.330(8) . ? N31 C36 1.363(7) . ? C32 C33 1.399(7) . ? C32 C37 1.501(8) . ? C33 N34 1.336(7) . ? C33 C38 1.490(9) . ? N34 C35 1.339(8) . ? N34 Ag1 2.307(4) 2_666 ? C35 C36 1.395(8) . ? C35 C39 1.501(8) . ? C36 C40 1.491(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? O1S C1S 1.435(11) . ? O1S H1SO 0.7986 . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C1S H1S3 0.9700 . ? 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 N34 Ag1 N21 120.41(14) 2_666 . ? N34 Ag1 O1S 125.60(18) 2_666 . ? N21 Ag1 O1S 101.73(16) . . ? N34 Ag1 O11B 92.76(18) 2_666 . ? N21 Ag1 O11B 123.04(18) . . ? O1S Ag1 O11B 91.1(2) . . ? N31 Ag2 O11A 129.81(18) . . ? N31 Ag2 O1B 119.83(16) . . ? O11A Ag2 O1B 107.58(18) . . ? C1 O1B Ag2 94.2(3) . . ? O1A C1 O1B 127.5(4) . . ? O1A C1 C2' 115.8(6) . . ? O1B C1 C2' 116.7(6) . . ? O1A C1 C2 118.2(6) . . ? O1B C1 C2 114.3(6) . . ? F2B C2 F2A 106.22(11) . . ? F2B C2 C3 108.2(6) . . ? F2A C2 C3 108.3(7) . . ? F2B C2 C1 116.0(7) . . ? F2A C2 C1 111.2(6) . . ? C3 C2 C1 106.8(5) . . ? F3A C3 F3B 106.37(11) . . ? F3A C3 C4 105.0(7) . . ? F3B C3 C4 101.7(7) . . ? F3A C3 C2 114.8(7) . . ? F3B C3 C2 112.5(7) . . ? C4 C3 C2 115.31(11) . . ? F4A C4 F4C 102.1(10) . . ? F4A C4 F4B 106.28(12) . . ? F4C C4 F4B 106.29(11) . . ? F4A C4 C3 113.2(7) . . ? F4C C4 C3 116.1(8) . . ? F4B C4 C3 111.9(7) . . ? F2Y C2' F2Z 106.27(11) . . ? F2Y C2' C1 108.7(7) . . ? F2Z C2' C1 111.1(8) . . ? F2Y C2' C3' 113.6(7) . . ? F2Z C2' C3' 107.5(7) . . ? C1 C2' C3' 109.7(6) . . ? F3Z C3' F3Y 106.25(11) . . ? F3Z C3' C4' 106.2(8) . . ? F3Y C3' C4' 106.8(8) . . ? F3Z C3' C2' 110.1(8) . . ? F3Y C3' C2' 111.8(9) . . ? C4' C3' C2' 115.14(11) . . ? F4Y C4' F4Z 106.38(12) . . ? F4Y C4' F4X 106.35(11) . . ? F4Z C4' F4X 111.4(12) . . ? F4Y C4' C3' 111.6(8) . . ? F4Z C4' C3' 112.2(8) . . ? F4X C4' C3' 108.7(8) . . ? C11 O11A Ag2 106.9(4) . . ? C11 O11B Ag1 164.5(6) . . ? O11B C11 O11A 129.0(5) . . ? O11B C11 C12' 114.0(7) . . ? O11A C11 C12' 117.0(6) . . ? O11B C11 C12 117.9(7) . . ? O11A C11 C12 113.0(6) . . ? F12B C12 F12A 106.22(11) . . ? F12B C12 C13 106.1(6) . . ? F12A C12 C13 100.3(6) . . ? F12B C12 C11 113.5(6) . . ? F12A C12 C11 113.4(6) . . ? C13 C12 C11 116.1(5) . . ? F13B C13 F13A 106.36(12) . . ? F13B C13 C14 100.1(8) . . ? F13A C13 C14 103.5(7) . . ? F13B C13 C12 112.1(8) . . ? F13A C13 C12 117.7(7) . . ? C14 C13 C12 115.24(12) . . ? F14B C14 F14C 106.32(12) . . ? F14B C14 F14A 106.30(11) . . ? F14C C14 F14A 102.1(10) . . ? F14B C14 C13 112.6(7) . . ? F14C C14 C13 112.8(7) . . ? F14A C14 C13 115.8(7) . . ? F12Y C12' F12Z 106.28(12) . . ? F12Y C12' C13' 106.5(8) . . ? F12Z C12' C13' 98.7(8) . . ? F12Y C12' C11 114.0(9) . . ? F12Z C12' C11 109.1(8) . . ? C13' C12' C11 120.4(7) . . ? F13Y C13' F13Z 106.29(12) . . ? F13Y C13' C14' 110.5(11) . . ? F13Z C13' C14' 101.4(10) . . ? F13Y C13' C12' 110.1(11) . . ? F13Z C13' C12' 112.7(10) . . ? C14' C13' C12' 115.20(12) . . ? F14Z C14' F14Y 106.33(12) . . ? F14Z C14' F14X 117.0(12) . . ? F14Y C14' F14X 106.31(12) . . ? F14Z C14' C13' 103.0(9) . . ? F14Y C14' C13' 103.1(11) . . ? F14X C14' C13' 119.6(10) . . ? C26 N21 C22 118.5(4) . . ? C26 N21 Ag1 120.5(3) . . ? C22 N21 Ag1 120.7(3) . . ? N21 C22 C26 121.5(4) . 2_777 ? N21 C22 C27 116.5(5) . . ? C26 C22 C27 122.0(5) 2_777 . ? N21 C26 C22 120.0(4) . 2_777 ? N21 C26 C28 117.4(5) . . ? C22 C26 C28 122.6(4) 2_777 . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 N31 C36 118.8(5) . . ? C32 N31 Ag2 120.4(4) . . ? C36 N31 Ag2 120.8(4) . . ? N31 C32 C33 121.4(5) . . ? N31 C32 C37 117.1(5) . . ? C33 C32 C37 121.5(5) . . ? N34 C33 C32 119.8(5) . . ? N34 C33 C38 118.6(5) . . ? C32 C33 C38 121.7(5) . . ? C33 N34 C35 119.5(5) . . ? C33 N34 Ag1 121.2(4) . 2_666 ? C35 N34 Ag1 118.8(3) . 2_666 ? N34 C35 C36 120.9(5) . . ? N34 C35 C39 117.2(5) . . ? C36 C35 C39 121.9(5) . . ? N31 C36 C35 119.6(5) . . ? N31 C36 C40 117.5(5) . . ? C35 C36 C40 122.9(5) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1S O1S Ag1 121.6(5) . . ? C1S O1S H1SO 114.1 . . ? Ag1 O1S H1SO 108.1 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 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 N31 Ag2 O1B C1 -103.3(4) . . . . ? O11A Ag2 O1B C1 93.8(4) . . . . ? Ag2 O1B C1 O1A -3.8(8) . . . . ? Ag2 O1B C1 C2' 176.9(5) . . . . ? Ag2 O1B C1 C2 177.0(5) . . . . ? O1A C1 C2 F2B -166.7(7) . . . . ? O1B C1 C2 F2B 12.7(9) . . . . ? C2' C1 C2 F2B -169(10) . . . . ? O1A C1 C2 F2A -45.2(8) . . . . ? O1B C1 C2 F2A 134.1(7) . . . . ? C2' C1 C2 F2A -48(9) . . . . ? O1A C1 C2 C3 72.7(8) . . . . ? O1B C1 C2 C3 -107.9(7) . . . . ? C2' C1 C2 C3 70(9) . . . . ? F2B C2 C3 F3A 165.7(7) . . . . ? F2A C2 C3 F3A 50.9(7) . . . . ? C1 C2 C3 F3A -68.9(8) . . . . ? F2B C2 C3 F3B -72.6(7) . . . . ? F2A C2 C3 F3B 172.7(7) . . . . ? C1 C2 C3 F3B 52.9(8) . . . . ? F2B C2 C3 C4 43.4(9) . . . . ? F2A C2 C3 C4 -71.3(8) . . . . ? C1 C2 C3 C4 168.9(6) . . . . ? F3A C3 C4 F4A -77.3(8) . . . . ? F3B C3 C4 F4A 172.1(7) . . . . ? C2 C3 C4 F4A 50.1(10) . . . . ? F3A C3 C4 F4C 165.1(8) . . . . ? F3B C3 C4 F4C 54.4(9) . . . . ? C2 C3 C4 F4C -67.6(10) . . . . ? F3A C3 C4 F4B 42.9(7) . . . . ? F3B C3 C4 F4B -67.8(7) . . . . ? C2 C3 C4 F4B 170.2(6) . . . . ? O1A C1 C2' F2Y -142.9(7) . . . . ? O1B C1 C2' F2Y 36.5(9) . . . . ? C2 C1 C2' F2Y 35(9) . . . . ? O1A C1 C2' F2Z -26.4(9) . . . . ? O1B C1 C2' F2Z 153.1(7) . . . . ? C2 C1 C2' F2Z 151(10) . . . . ? O1A C1 C2' C3' 92.3(8) . . . . ? O1B C1 C2' C3' -88.2(9) . . . . ? C2 C1 C2' C3' -90(10) . . . . ? F2Y C2' C3' F3Z -59.3(8) . . . . ? F2Z C2' C3' F3Z -176.6(8) . . . . ? C1 C2' C3' F3Z 62.5(9) . . . . ? F2Y C2' C3' F3Y -177.2(8) . . . . ? F2Z C2' C3' F3Y 65.5(8) . . . . ? C1 C2' C3' F3Y -55.4(10) . . . . ? F2Y C2' C3' C4' 60.6(10) . . . . ? F2Z C2' C3' C4' -56.6(10) . . . . ? C1 C2' C3' C4' -177.5(7) . . . . ? F3Z C3' C4' F4Y -56.1(8) . . . . ? F3Y C3' C4' F4Y 57.0(9) . . . . ? C2' C3' C4' F4Y -178.2(7) . . . . ? F3Z C3' C4' F4Z -175.4(9) . . . . ? F3Y C3' C4' F4Z -62.3(10) . . . . ? C2' C3' C4' F4Z 62.5(11) . . . . ? F3Z C3' C4' F4X 60.9(10) . . . . ? F3Y C3' C4' F4X 174.0(8) . . . . ? C2' C3' C4' F4X -61.2(11) . . . . ? N31 Ag2 O11A C11 -87.6(5) . . . . ? O1B Ag2 O11A C11 73.0(5) . . . . ? N34 Ag1 O11B C11 138.1(19) 2_666 . . . ? N21 Ag1 O11B C11 -92.4(19) . . . . ? O1S Ag1 O11B C11 12.4(19) . . . . ? Ag1 O11B C11 O11A -80(2) . . . . ? Ag1 O11B C11 C12' 99.9(19) . . . . ? Ag1 O11B C11 C12 97.3(19) . . . . ? Ag2 O11A C11 O11B -2.9(11) . . . . ? Ag2 O11A C11 C12' 177.4(6) . . . . ? Ag2 O11A C11 C12 180.0(5) . . . . ? O11B C11 C12 F12B -152.4(8) . . . . ? O11A C11 C12 F12B 25.1(9) . . . . ? C12' C11 C12 F12B 175(6) . . . . ? O11B C11 C12 F12A -31.1(10) . . . . ? O11A C11 C12 F12A 146.4(7) . . . . ? C12' C11 C12 F12A -63(5) . . . . ? O11B C11 C12 C13 84.3(8) . . . . ? O11A C11 C12 C13 -98.2(7) . . . . ? C12' C11 C12 C13 52(5) . . . . ? F12B C12 C13 F13B -174.0(7) . . . . ? F12A C12 C13 F13B 75.7(7) . . . . ? C11 C12 C13 F13B -46.9(8) . . . . ? F12B C12 C13 F13A 62.2(8) . . . . ? F12A C12 C13 F13A -48.1(8) . . . . ? C11 C12 C13 F13A -170.7(7) . . . . ? F12B C12 C13 C14 -60.4(8) . . . . ? F12A C12 C13 C14 -170.7(7) . . . . ? C11 C12 C13 C14 66.6(9) . . . . ? F13B C13 C14 F14B 56.2(6) . . . . ? F13A C13 C14 F14B 165.9(6) . . . . ? C12 C13 C14 F14B -64.2(8) . . . . ? F13B C13 C14 F14C 176.5(7) . . . . ? F13A C13 C14 F14C -73.8(7) . . . . ? C12 C13 C14 F14C 56.1(10) . . . . ? F13B C13 C14 F14A -66.4(9) . . . . ? F13A C13 C14 F14A 43.3(10) . . . . ? C12 C13 C14 F14A 173.2(7) . . . . ? O11B C11 C12' F12Y -6.7(11) . . . . ? O11A C11 C12' F12Y 173.1(8) . . . . ? C12 C11 C12' F12Y 142(6) . . . . ? O11B C11 C12' F12Z -125.3(9) . . . . ? O11A C11 C12' F12Z 54.4(10) . . . . ? C12 C11 C12' F12Z 23(5) . . . . ? O11B C11 C12' C13' 121.8(9) . . . . ? O11A C11 C12' C13' -58.5(10) . . . . ? C12 C11 C12' C13' -89(6) . . . . ? F12Y C12' C13' F13Y -164.4(9) . . . . ? F12Z C12' C13' F13Y -54.4(10) . . . . ? C11 C12' C13' F13Y 63.9(10) . . . . ? F12Y C12' C13' F13Z -45.9(10) . . . . ? F12Z C12' C13' F13Z 64.0(10) . . . . ? C11 C12' C13' F13Z -177.6(9) . . . . ? F12Y C12' C13' C14' 69.9(11) . . . . ? F12Z C12' C13' C14' 179.8(10) . . . . ? C11 C12' C13' C14' -61.9(12) . . . . ? F13Y C13' C14' F14Z -68.2(9) . . . . ? F13Z C13' C14' F14Z 179.4(9) . . . . ? C12' C13' C14' F14Z 57.3(11) . . . . ? F13Y C13' C14' F14Y -178.7(9) . . . . ? F13Z C13' C14' F14Y 68.9(9) . . . . ? C12' C13' C14' F14Y -53.2(10) . . . . ? F13Y C13' C14' F14X 63.6(14) . . . . ? F13Z C13' C14' F14X -48.8(12) . . . . ? C12' C13' C14' F14X -170.9(10) . . . . ? N34 Ag1 N21 C26 -27.6(4) 2_666 . . . ? O1S Ag1 N21 C26 116.6(4) . . . . ? O11B Ag1 N21 C26 -144.2(4) . . . . ? N34 Ag1 N21 C22 146.6(4) 2_666 . . . ? O1S Ag1 N21 C22 -69.2(4) . . . . ? O11B Ag1 N21 C22 29.9(5) . . . . ? C26 N21 C22 C26 0.1(9) . . . 2_777 ? Ag1 N21 C22 C26 -174.2(4) . . . 2_777 ? C26 N21 C22 C27 -179.2(5) . . . . ? Ag1 N21 C22 C27 6.6(7) . . . . ? C22 N21 C26 C22 -0.1(9) . . . 2_777 ? Ag1 N21 C26 C22 174.2(4) . . . 2_777 ? C22 N21 C26 C28 179.4(5) . . . . ? Ag1 N21 C26 C28 -6.3(6) . . . . ? O11A Ag2 N31 C32 18.6(5) . . . . ? O1B Ag2 N31 C32 -140.0(4) . . . . ? O11A Ag2 N31 C36 -160.7(4) . . . . ? O1B Ag2 N31 C36 40.6(4) . . . . ? C36 N31 C32 C33 0.9(8) . . . . ? Ag2 N31 C32 C33 -178.5(4) . . . . ? C36 N31 C32 C37 177.9(5) . . . . ? Ag2 N31 C32 C37 -1.5(7) . . . . ? N31 C32 C33 N34 -2.1(8) . . . . ? C37 C32 C33 N34 -178.9(5) . . . . ? N31 C32 C33 C38 177.4(5) . . . . ? C37 C32 C33 C38 0.6(8) . . . . ? C32 C33 N34 C35 1.8(7) . . . . ? C38 C33 N34 C35 -177.7(5) . . . . ? C32 C33 N34 Ag1 173.6(4) . . . 2_666 ? C38 C33 N34 Ag1 -5.9(7) . . . 2_666 ? C33 N34 C35 C36 -0.4(8) . . . . ? Ag1 N34 C35 C36 -172.4(4) 2_666 . . . ? C33 N34 C35 C39 179.2(5) . . . . ? Ag1 N34 C35 C39 7.2(6) 2_666 . . . ? C32 N31 C36 C35 0.4(8) . . . . ? Ag2 N31 C36 C35 179.8(4) . . . . ? C32 N31 C36 C40 -178.3(5) . . . . ? Ag2 N31 C36 C40 1.1(7) . . . . ? N34 C35 C36 N31 -0.7(8) . . . . ? C39 C35 C36 N31 179.7(5) . . . . ? N34 C35 C36 C40 177.9(5) . . . . ? C39 C35 C36 C40 -1.7(9) . . . . ? N34 Ag1 O1S C1S 93.5(6) 2_666 . . . ? N21 Ag1 O1S C1S -48.1(6) . . . . ? O11B Ag1 O1S C1S -172.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.187 _refine_diff_density_min -1.280 _refine_diff_density_rms 0.151 data_ilb1119_0m _database_code_depnum_ccdc_archive 'CCDC 903743' #TrackingRef 'SCSC1_step1_1_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 Ag4 F28 N6 O8' _chemical_formula_weight 1692.18 _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5244(2) _cell_length_b 12.9043(2) _cell_length_c 14.8417(3) _cell_angle_alpha 112.5240(10) _cell_angle_beta 90.4820(10) _cell_angle_gamma 109.2510(10) _cell_volume 1406.65(5) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 9945 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 23.93 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method ? _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 1.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6945 _exptl_absorpt_correction_T_max 0.9147 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33666 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.43 _reflns_number_total 6366 _reflns_number_gt 4232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6366 _refine_ls_number_parameters 376 _refine_ls_number_restraints 294 _refine_ls_R_factor_all 0.1064 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.3084 _refine_ls_wR_factor_gt 0.2620 _refine_ls_goodness_of_fit_ref 1.195 _refine_ls_restrained_S_all 1.231 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.57285(8) 0.42921(6) 0.20791(5) 0.0642(3) Uani 1 1 d . . . Ag2 Ag 0.89275(9) 0.48462(6) 0.37672(4) 0.0664(3) Uani 1 1 d . . . O1A O 0.9316(9) 0.3149(7) 0.2645(6) 0.0883(16) Uani 1 1 d U A . O1B O 0.6866(9) 0.2821(7) 0.1869(6) 0.0948(16) Uani 1 1 d U A . C1 C 0.8050(14) 0.2556(7) 0.1984(7) 0.0879(14) Uani 1 1 d DU . . C2 C 0.8003(13) 0.1321(6) 0.1238(7) 0.0995(16) Uiso 0.512(8) 1 d PDU A 1 F2A F 0.9497(14) 0.1174(12) 0.1257(9) 0.090(3) Uiso 0.512(8) 1 d PDU A 1 F2B F 0.7686(17) 0.1362(14) 0.0361(9) 0.107(3) Uiso 0.512(8) 1 d PDU A 1 C3 C 0.7150(14) 0.0305(9) 0.1572(6) 0.1126(17) Uiso 0.512(8) 1 d PDU A 1 F3A F 0.8155(14) 0.0584(13) 0.2404(9) 0.112(3) Uiso 0.512(8) 1 d PDU A 1 F3B F 0.5604(13) 0.0207(15) 0.1819(11) 0.124(3) Uiso 0.512(8) 1 d PDU A 1 C4 C 0.7192(13) -0.0936(7) 0.0901(10) 0.123(2) Uiso 0.512(8) 1 d PDU A 1 F4A F 0.8802(15) -0.0837(16) 0.0807(13) 0.132(3) Uiso 0.512(8) 1 d PDU A 1 F4B F 0.665(2) -0.1658(14) 0.1382(11) 0.136(3) Uiso 0.512(8) 1 d PDU A 1 F4C F 0.6057(19) -0.1412(15) 0.0077(10) 0.136(3) Uiso 0.512(8) 1 d PDU A 1 C2' C 0.8081(13) 0.1339(6) 0.1248(6) 0.0995(16) Uiso 0.488(8) 1 d PDU A 2 F2Y F 0.7073(12) 0.0896(14) 0.0378(10) 0.100(3) Uiso 0.488(8) 1 d PDU A 2 F2Z F 0.9660(11) 0.1511(12) 0.1039(9) 0.088(3) Uiso 0.488(8) 1 d PDU A 2 C3' C 0.6989(14) 0.0325(9) 0.1529(7) 0.1127(18) Uiso 0.488(8) 1 d PDU A 2 F3Y F 0.7230(18) 0.0625(14) 0.2510(7) 0.113(3) Uiso 0.488(8) 1 d PDU A 2 F3Z F 0.5424(16) 0.0281(15) 0.1304(10) 0.116(3) Uiso 0.488(8) 1 d PDU A 2 C4' C 0.6944(14) -0.0943(8) 0.0866(9) 0.123(2) Uiso 0.488(8) 1 d PDU A 2 F4X F 0.701(2) -0.1047(16) -0.0073(9) 0.132(3) Uiso 0.488(8) 1 d PDU A 2 F4Y F 0.8280(15) -0.1163(16) 0.1130(12) 0.134(3) Uiso 0.488(8) 1 d PDU A 2 F4Z F 0.5589(16) -0.1667(14) 0.1076(15) 0.143(3) Uiso 0.488(8) 1 d PDU A 2 O11A O 1.0870(8) 0.6317(6) 0.3315(5) 0.0802(15) Uani 1 1 d U B . O11B O 0.8375(8) 0.6118(7) 0.2737(5) 0.0887(16) Uani 1 1 d U B . C11 C 0.9927(12) 0.6547(8) 0.2870(7) 0.0819(14) Uani 1 1 d DU . . C12 C 1.0884(8) 0.7462(5) 0.2454(4) 0.0894(15) Uiso 0.600(9) 1 d PDU B 1 F12A F 1.2438(9) 0.7438(9) 0.2319(7) 0.087(2) Uiso 0.600(9) 1 d PDU B 1 F12B F 1.0111(12) 0.7251(10) 0.1571(6) 0.097(2) Uiso 0.600(9) 1 d PDU B 1 C13 C 1.1184(9) 0.8792(6) 0.3098(5) 0.1003(17) Uiso 0.600(9) 1 d PDU B 1 F13A F 0.9700(11) 0.8955(11) 0.3206(10) 0.117(3) Uiso 0.600(9) 1 d PDU B 1 F13B F 1.2023(14) 0.9485(10) 0.2641(9) 0.110(3) Uiso 0.600(9) 1 d PDU B 1 C14 C 1.2476(9) 0.9369(5) 0.4044(5) 0.105(2) Uiso 0.600(9) 1 d PDU B 1 F14A F 1.1863(15) 0.8854(8) 0.4668(5) 0.114(3) Uiso 0.600(9) 1 d PDU B 1 F14B F 1.2691(13) 1.0543(5) 0.4513(7) 0.120(3) Uiso 0.600(9) 1 d PDU B 1 F14C F 1.3983(9) 0.9330(10) 0.3800(7) 0.136(3) Uiso 0.600(9) 1 d PDU B 1 C12' C 1.0631(14) 0.7545(6) 0.2496(5) 0.0892(16) Uiso 0.400(9) 1 d PDU B 2 F12Y F 1.1979(15) 0.7460(15) 0.2044(11) 0.093(3) Uiso 0.400(9) 1 d PDU B 2 F12Z F 0.9421(16) 0.7356(15) 0.1797(10) 0.098(3) Uiso 0.400(9) 1 d PDU B 2 C13' C 1.0922(14) 0.8863(7) 0.3169(6) 0.1002(17) Uiso 0.400(9) 1 d PDU B 2 F13Y F 1.100(2) 0.9586(14) 0.2698(12) 0.114(3) Uiso 0.400(9) 1 d PDU B 2 F13Z F 0.962(2) 0.8882(16) 0.3678(13) 0.115(3) Uiso 0.400(9) 1 d PDU B 2 C14' C 1.1898(12) 0.9332(7) 0.4209(6) 0.104(2) Uiso 0.400(9) 1 d PDU B 2 F14X F 1.3311(14) 0.9067(13) 0.4133(9) 0.116(3) Uiso 0.400(9) 1 d PDU B 2 F14Z F 1.2111(19) 1.0502(8) 0.4709(8) 0.110(3) Uiso 0.400(9) 1 d PDU B 2 F14Y F 1.097(2) 0.8742(12) 0.4715(7) 0.117(4) Uiso 0.400(9) 1 d PDU B 2 N21 N 0.7634(7) 0.5133(5) 0.5118(4) 0.0482(11) Uani 1 1 d U . . C22 C 0.7708(9) 0.6218(6) 0.5723(5) 0.0477(11) Uani 1 1 d U . . C23 C 0.6836(8) 0.6370(6) 0.6509(5) 0.0464(11) Uani 1 1 d U . . N24 N 0.5866(7) 0.5430(5) 0.6683(4) 0.0475(11) Uani 1 1 d U . . C25 C 0.5834(9) 0.4318(6) 0.6091(5) 0.0516(12) Uani 1 1 d U . . C26 C 0.6697(9) 0.4168(6) 0.5291(5) 0.0521(12) Uani 1 1 d U . . C27 C 0.8831(10) 0.7242(7) 0.5536(6) 0.0614(17) Uani 1 1 d U . . H27A H 0.9762 0.7727 0.6076 0.092 Uiso 1 1 calc R . . H27B H 0.8206 0.7730 0.5487 0.092 Uiso 1 1 calc R . . H27C H 0.9261 0.6940 0.4924 0.092 Uiso 1 1 calc R . . C28 C 0.6950(11) 0.7607(7) 0.7253(6) 0.0619(18) Uani 1 1 d U . . H28A H 0.6077 0.7517 0.7662 0.093 Uiso 1 1 calc R . . H28B H 0.6803 0.8077 0.6905 0.093 Uiso 1 1 calc R . . H28C H 0.8043 0.8014 0.7666 0.093 Uiso 1 1 calc R . . C29 C 0.4840(10) 0.3303(7) 0.6332(6) 0.0604(17) Uani 1 1 d U . . H29A H 0.5587 0.2964 0.6515 0.091 Uiso 1 1 calc R . . H29B H 0.4026 0.2690 0.5760 0.091 Uiso 1 1 calc R . . H29C H 0.4256 0.3589 0.6878 0.091 Uiso 1 1 calc R . . C30 C 0.6620(11) 0.2952(7) 0.4601(6) 0.067(2) Uani 1 1 d U . . H30A H 0.7319 0.3024 0.4099 0.100 Uiso 1 1 calc R . . H30B H 0.5467 0.2457 0.4288 0.100 Uiso 1 1 calc R . . H30C H 0.7025 0.2583 0.4965 0.100 Uiso 1 1 calc R . . N31 N 0.5088(7) 0.4492(5) 0.0651(4) 0.0480(11) Uani 1 1 d U . . C32 C 0.3739(8) 0.4776(6) 0.0519(5) 0.0489(13) Uani 1 1 d U . . C36 C 0.6330(8) 0.4706(7) 0.0126(5) 0.0497(13) Uani 1 1 d U . . C37 C 0.2328(9) 0.4450(8) 0.1080(6) 0.0590(17) Uani 1 1 d U . . H37A H 0.2523 0.3941 0.1375 0.089 Uiso 1 1 calc R . . H37B H 0.1270 0.4021 0.0632 0.089 Uiso 1 1 calc R . . H37C H 0.2282 0.5177 0.1596 0.089 Uiso 1 1 calc R . . C40 C 0.7782(9) 0.4337(8) 0.0248(6) 0.0591(17) Uani 1 1 d U . . H40A H 0.8799 0.5045 0.0531 0.089 Uiso 1 1 calc R . . H40B H 0.7921 0.3805 -0.0391 0.089 Uiso 1 1 calc R . . H40C H 0.7566 0.3921 0.0683 0.089 Uiso 1 1 calc R . . _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 0.0669(5) 0.0827(5) 0.0644(4) 0.0419(4) 0.0241(3) 0.0388(4) Ag2 0.0778(5) 0.0697(5) 0.0545(4) 0.0258(3) 0.0188(3) 0.0292(4) O1A 0.096(3) 0.090(3) 0.089(3) 0.032(2) 0.011(3) 0.053(2) O1B 0.094(3) 0.093(3) 0.114(3) 0.042(3) 0.011(3) 0.055(2) C1 0.093(2) 0.091(2) 0.096(2) 0.0422(18) 0.0126(18) 0.0496(18) O11A 0.075(3) 0.086(3) 0.085(3) 0.038(2) 0.012(2) 0.030(2) O11B 0.071(3) 0.090(3) 0.093(3) 0.033(2) 0.008(2) 0.020(2) C11 0.078(2) 0.085(2) 0.085(2) 0.0374(18) 0.0120(17) 0.0298(18) N21 0.047(2) 0.050(2) 0.046(2) 0.0211(17) 0.0020(18) 0.0143(18) C22 0.048(2) 0.050(2) 0.048(2) 0.0231(18) 0.0017(19) 0.0167(18) C23 0.047(2) 0.049(2) 0.048(2) 0.0237(18) 0.0015(18) 0.0189(18) N24 0.043(2) 0.050(2) 0.050(2) 0.0209(18) -0.0007(18) 0.0164(17) C25 0.046(2) 0.053(2) 0.052(2) 0.0210(19) 0.0009(19) 0.0124(19) C26 0.049(2) 0.051(2) 0.051(2) 0.0196(19) -0.0006(19) 0.0136(19) C27 0.065(4) 0.055(3) 0.061(4) 0.027(3) 0.014(3) 0.014(3) C28 0.062(4) 0.052(3) 0.061(4) 0.019(3) 0.008(3) 0.014(3) C29 0.056(4) 0.052(3) 0.066(4) 0.021(3) 0.011(3) 0.013(3) C30 0.070(4) 0.049(3) 0.066(4) 0.015(3) 0.006(3) 0.012(3) N31 0.042(2) 0.060(2) 0.047(2) 0.0221(18) 0.0085(18) 0.0237(19) C32 0.041(2) 0.061(3) 0.046(2) 0.020(2) 0.011(2) 0.023(2) C36 0.042(2) 0.063(3) 0.047(2) 0.021(2) 0.010(2) 0.024(2) C37 0.047(3) 0.076(4) 0.060(3) 0.033(3) 0.019(3) 0.023(3) C40 0.049(3) 0.080(4) 0.057(3) 0.030(3) 0.014(3) 0.031(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. ; _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 N24 2.283(6) 2_666 ? Ag1 N31 2.312(6) . ? Ag1 O1B 2.325(6) . ? Ag1 O11B 2.508(7) . ? Ag2 N21 2.261(6) . ? Ag2 O1A 2.318(7) . ? Ag2 O11A 2.391(7) . ? O1A C1 1.255(12) . ? O1B C1 1.197(11) . ? C1 C2' 1.5400(11) . ? C1 C2 1.5401(11) . ? C2 F2A 1.3500(11) . ? C2 F2B 1.3503(11) . ? C2 C3 1.5401(11) . ? C3 F3A 1.3499(11) . ? C3 F3B 1.3502(11) . ? C3 C4 1.5401(11) . ? C4 F4A 1.3501(11) . ? C4 F4C 1.3501(11) . ? C4 F4B 1.3501(11) . ? C2' F2Y 1.3502(11) . ? C2' F2Z 1.3501(11) . ? C2' C3' 1.5400(11) . ? C3' F3Y 1.3500(11) . ? C3' F3Z 1.3502(11) . ? C3' C4' 1.5401(11) . ? C4' F4X 1.3501(11) . ? C4' F4Z 1.3501(11) . ? C4' F4Y 1.3501(11) . ? O11A C11 1.212(11) . ? O11B C11 1.235(11) . ? C11 C12' 1.5398(11) . ? C11 C12 1.5400(11) . ? C12 F12B 1.3496(11) . ? C12 F12A 1.3503(11) . ? C12 C13 1.5402(11) . ? C13 F13A 1.3500(11) . ? C13 F13B 1.3503(11) . ? C13 C14 1.5394(11) . ? C14 F14B 1.3487(11) . ? C14 F14C 1.3493(11) . ? C14 F14A 1.3492(11) . ? C12' F12Y 1.3500(11) . ? C12' F12Z 1.3503(11) . ? C12' C13' 1.5392(11) . ? C13' F13Y 1.3494(11) . ? C13' F13Z 1.3498(11) . ? C13' C14' 1.5395(11) . ? C14' F14X 1.3500(11) . ? C14' F14Z 1.3504(11) . ? C14' F14Y 1.3503(11) . ? N21 C22 1.322(9) . ? N21 C26 1.359(10) . ? C22 C23 1.374(10) . ? C22 C27 1.480(10) . ? C23 N24 1.343(9) . ? C23 C28 1.524(10) . ? N24 C25 1.356(9) . ? N24 Ag1 2.283(6) 2_666 ? C25 C26 1.387(11) . ? C25 C29 1.482(11) . ? C26 C30 1.488(11) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? N31 C32 1.351(8) . ? N31 C36 1.339(9) . ? C32 C36 1.370(10) 2_665 ? C32 C37 1.507(10) . ? C36 C32 1.370(10) 2_665 ? C36 C40 1.498(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? _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 N24 Ag1 N31 121.83(18) 2_666 . ? N24 Ag1 O1B 114.2(3) 2_666 . ? N31 Ag1 O1B 115.1(2) . . ? N24 Ag1 O11B 104.7(2) 2_666 . ? N31 Ag1 O11B 95.9(2) . . ? O1B Ag1 O11B 99.3(3) . . ? N21 Ag2 O1A 131.2(3) . . ? N21 Ag2 O11A 128.7(2) . . ? O1A Ag2 O11A 98.6(3) . . ? C1 O1A Ag2 108.7(5) . . ? C1 O1B Ag1 149.6(7) . . ? O1B C1 O1A 128.2(7) . . ? O1B C1 C2' 118.2(9) . . ? O1A C1 C2' 113.5(8) . . ? O1B C1 C2 116.1(9) . . ? O1A C1 C2 115.7(8) . . ? F2A C2 F2B 106.25(11) . . ? F2A C2 C3 93.1(9) . . ? F2B C2 C3 128.5(11) . . ? F2A C2 C1 113.7(9) . . ? F2B C2 C1 102.5(9) . . ? C3 C2 C1 112.6(8) . . ? F3A C3 F3B 106.25(11) . . ? F3A C3 C4 101.9(11) . . ? F3B C3 C4 110.8(10) . . ? F3A C3 C2 104.8(11) . . ? F3B C3 C2 116.3(11) . . ? C4 C3 C2 115.17(11) . . ? F4A C4 F4C 118.8(14) . . ? F4A C4 F4B 106.26(11) . . ? F4C C4 F4B 106.23(11) . . ? F4A C4 C3 109.1(10) . . ? F4C C4 C3 108.9(11) . . ? F4B C4 C3 107.0(11) . . ? F2Y C2' F2Z 106.26(11) . . ? F2Y C2' C1 113.3(11) . . ? F2Z C2' C1 107.9(9) . . ? F2Y C2' C3' 92.7(10) . . ? F2Z C2' C3' 126.0(10) . . ? C1 C2' C3' 109.7(8) . . ? F3Y C3' F3Z 106.24(11) . . ? F3Y C3' C2' 112.5(10) . . ? F3Z C3' C2' 101.9(11) . . ? F3Y C3' C4' 115.6(11) . . ? F3Z C3' C4' 103.6(10) . . ? C2' C3' C4' 115.17(11) . . ? F4X C4' F4Z 119.7(14) . . ? F4X C4' F4Y 106.25(11) . . ? F4Z C4' F4Y 106.23(11) . . ? F4X C4' C3' 109.4(9) . . ? F4Z C4' C3' 102.9(10) . . ? F4Y C4' C3' 112.5(13) . . ? C11 O11A Ag2 101.5(5) . . ? C11 O11B Ag1 148.6(7) . . ? O11A C11 O11B 126.3(7) . . ? O11A C11 C12' 120.2(8) . . ? O11B C11 C12' 113.3(9) . . ? O11A C11 C12 112.2(8) . . ? O11B C11 C12 121.5(8) . . ? F12B C12 F12A 106.28(11) . . ? F12B C12 C11 113.1(7) . . ? F12A C12 C11 111.2(8) . . ? F12B C12 C13 104.6(6) . . ? F12A C12 C13 104.5(6) . . ? C11 C12 C13 116.3(6) . . ? F13A C13 F13B 106.24(11) . . ? F13A C13 C14 116.4(8) . . ? F13B C13 C14 98.0(7) . . ? F13A C13 C12 110.1(7) . . ? F13B C13 C12 109.8(7) . . ? C14 C13 C12 115.15(11) . . ? F14B C14 F14C 106.39(11) . . ? F14B C14 F14A 106.42(11) . . ? F14C C14 F14A 115.6(3) . . ? F14B C14 C13 109.45(11) . . ? F14C C14 C13 109.39(11) . . ? F14A C14 C13 109.41(11) . . ? F12Y C12' F12Z 106.24(11) . . ? F12Y C12' C13' 110.8(10) . . ? F12Z C12' C13' 99.1(9) . . ? F12Y C12' C11 111.8(10) . . ? F12Z C12' C11 106.5(10) . . ? C13' C12' C11 120.6(7) . . ? F13Y C13' F13Z 106.33(11) . . ? F13Y C13' C14' 122.4(10) . . ? F13Z C13' C14' 82.0(10) . . ? F13Y C13' C12' 115.3(9) . . ? F13Z C13' C12' 108.2(12) . . ? C14' C13' C12' 115.30(11) . . ? F14X C14' F14Z 116.2(3) . . ? F14X C14' F14Y 106.25(11) . . ? F14Z C14' F14Y 106.20(11) . . ? F14X C14' C13' 109.36(11) . . ? F14Z C14' C13' 109.30(11) . . ? F14Y C14' C13' 109.32(11) . . ? C22 N21 C26 119.1(6) . . ? C22 N21 Ag2 121.4(5) . . ? C26 N21 Ag2 119.5(5) . . ? N21 C22 C23 120.7(6) . . ? N21 C22 C27 116.7(6) . . ? C23 C22 C27 122.6(6) . . ? N24 C23 C22 121.6(6) . . ? N24 C23 C28 115.9(6) . . ? C22 C23 C28 122.5(6) . . ? C23 N24 C25 118.2(6) . . ? C23 N24 Ag1 120.4(4) . 2_666 ? C25 N24 Ag1 121.4(5) . 2_666 ? N24 C25 C26 119.8(7) . . ? N24 C25 C29 117.4(7) . . ? C26 C25 C29 122.7(7) . . ? N21 C26 C25 120.5(7) . . ? N21 C26 C30 118.5(7) . . ? C25 C26 C30 121.0(7) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 N31 C36 118.4(6) . . ? C32 N31 Ag1 120.8(4) . . ? C36 N31 Ag1 117.4(4) . . ? N31 C32 C36 120.4(6) . 2_665 ? N31 C32 C37 116.5(6) . . ? C36 C32 C37 123.1(6) 2_665 . ? N31 C36 C32 121.2(6) . 2_665 ? N31 C36 C40 117.8(6) . . ? C32 C36 C40 121.0(6) 2_665 . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.200 _refine_diff_density_min -1.444 _refine_diff_density_rms 0.151 data_ilb1120 _database_code_depnum_ccdc_archive 'CCDC 903744' #TrackingRef 'SCSC1_step2(end)_1-MeOH_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Ag4 F28 N6 O10' _chemical_formula_weight 1756.31 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8394(4) _cell_length_b 12.3968(5) _cell_length_c 15.1322(7) _cell_angle_alpha 109.787(3) _cell_angle_beta 97.080(3) _cell_angle_gamma 104.220(3) _cell_volume 1473.24(11) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 8921 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description 'BLOCK FROM A NEEDLE' _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 1.455 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6861 _exptl_absorpt_correction_T_max 0.8925 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25336 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6456 _reflns_number_gt 2955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+14.8373P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6456 _refine_ls_number_parameters 395 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1851 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2610 _refine_ls_wR_factor_gt 0.1909 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.85636(11) 0.22454(9) 0.18366(7) 0.0563(3) Uani 1 1 d . . . Ag2 Ag 0.69059(14) 0.59839(10) 0.62792(8) 0.0681(4) Uani 1 1 d . . . N21 N 0.7502(11) 0.4824(8) 0.4939(7) 0.047(2) Uani 1 1 d . . . N24 N 0.8234(9) 0.3451(8) 0.3301(6) 0.041(2) Uani 1 1 d . . . C23 C 0.8649(11) 0.4656(9) 0.3577(8) 0.039(2) Uani 1 1 d . . . C22 C 0.8301(12) 0.5340(10) 0.4409(8) 0.044(3) Uani 1 1 d . . . C26 C 0.7072(12) 0.3625(10) 0.4652(8) 0.043(3) Uani 1 1 d . . . C25 C 0.7446(12) 0.2924(10) 0.3820(8) 0.041(2) Uani 1 1 d . . . C29 C 0.7014(15) 0.1567(10) 0.3474(10) 0.058(3) Uani 1 1 d . . . H29A H 0.5857 0.1217 0.3293 0.086 Uiso 1 1 calc R . . H29B H 0.7447 0.1350 0.3987 0.086 Uiso 1 1 calc R . . H29C H 0.7461 0.1265 0.2920 0.086 Uiso 1 1 calc R . . C28 C 0.9437(14) 0.5198(12) 0.2943(9) 0.058(3) Uani 1 1 d . . . H28A H 1.0256 0.5955 0.3338 0.088 Uiso 1 1 calc R . . H28B H 0.8643 0.5343 0.2532 0.088 Uiso 1 1 calc R . . H28C H 0.9925 0.4649 0.2546 0.088 Uiso 1 1 calc R . . C27 C 0.8675(16) 0.6694(10) 0.4730(9) 0.057(3) Uani 1 1 d . . . H27A H 0.7890 0.6874 0.4342 0.086 Uiso 1 1 calc R . . H27B H 0.9736 0.7036 0.4650 0.086 Uiso 1 1 calc R . . H27C H 0.8640 0.7038 0.5403 0.086 Uiso 1 1 calc R . . C30 C 0.6173(16) 0.3068(11) 0.5241(10) 0.062(3) Uani 1 1 d . . . H30A H 0.6846 0.2737 0.5562 0.092 Uiso 1 1 calc R . . H30B H 0.5217 0.2429 0.4825 0.092 Uiso 1 1 calc R . . H30C H 0.5871 0.3676 0.5720 0.092 Uiso 1 1 calc R . . N31 N 0.6349(9) 0.0854(8) 0.0646(6) 0.045(2) Uani 1 1 d . . . C37 C 0.8061(13) -0.0353(12) 0.0110(10) 0.065(4) Uani 1 1 d . . . H37A H 0.8868 0.0429 0.0431 0.097 Uiso 1 1 calc R . . H37B H 0.8209 -0.0737 -0.0534 0.097 Uiso 1 1 calc R . . H37C H 0.8161 -0.0852 0.0474 0.097 Uiso 1 1 calc R . . C36 C 0.4925(11) 0.1057(9) 0.0595(7) 0.038(2) Uani 1 1 d . . . C40 C 0.4860(14) 0.2259(10) 0.1271(9) 0.057(3) Uani 1 1 d . . . H40A H 0.4690 0.2205 0.1878 0.086 Uiso 1 1 calc R . . H40B H 0.3984 0.2463 0.0983 0.086 Uiso 1 1 calc R . . H40C H 0.5862 0.2876 0.1385 0.086 Uiso 1 1 calc R . . C32 C 0.6420(12) -0.0196(10) 0.0044(7) 0.040(2) Uani 1 1 d . . . O1S O 1.0282(10) 0.2892(9) 0.0900(7) 0.069(3) Uani 1 1 d . . . H1SO H 1.1073 0.3389 0.1257 0.103 Uiso 1 1 d R . . C1S C 0.977(2) 0.3266(17) 0.0187(13) 0.101(6) Uani 1 1 d . . . H1S1 H 0.8759 0.2689 -0.0222 0.151 Uiso 1 1 calc R . . H1S2 H 1.0562 0.3322 -0.0198 0.151 Uiso 1 1 calc R . . H1S3 H 0.9621 0.4049 0.0480 0.151 Uiso 1 1 calc R . . O1A O 0.4626(10) 0.4973(8) 0.6976(7) 0.065(2) Uani 1 1 d . A . O1B O 0.7165(9) 0.5520(8) 0.7730(6) 0.063(2) Uani 1 1 d . A . C1 C 0.5697(15) 0.5049(10) 0.7584(8) 0.056(3) Uani 1 1 d D . . F2B F 0.3718(14) 0.4564(13) 0.8422(11) 0.072(4) Uiso 0.609(11) 1 d PDU A 1 F2A F 0.6124(17) 0.5106(13) 0.9187(9) 0.076(4) Uiso 0.609(11) 1 d PDU A 1 C2 C 0.5172(14) 0.4470(12) 0.8295(8) 0.057(4) Uiso 0.609(11) 1 d PDU A 1 F4A F 0.5537(15) 0.2937(15) 0.9412(12) 0.127(6) Uiso 0.609(11) 1 d PDU A 1 F3B F 0.386(2) 0.2508(18) 0.7013(13) 0.129(6) Uiso 0.609(11) 1 d PDU A 1 F3A F 0.6533(18) 0.3060(16) 0.7845(13) 0.108(5) Uiso 0.609(11) 1 d PDU A 1 F4B F 0.3112(14) 0.2526(15) 0.8771(13) 0.118(5) Uiso 0.609(11) 1 d PDU A 1 F4C F 0.441(2) 0.1358(15) 0.8181(13) 0.141(8) Uiso 0.609(11) 1 d PD A 1 C3 C 0.5027(18) 0.3125(12) 0.7824(10) 0.113(7) Uiso 0.609(11) 1 d PDU A 1 C4 C 0.4541(16) 0.2541(13) 0.8539(10) 0.110(7) Uiso 0.609(11) 1 d PDU A 1 C2' C 0.528(2) 0.4674(11) 0.8417(9) 0.059(4) Uiso 0.391(11) 1 d PDU A 2 C3' C 0.483(3) 0.3290(11) 0.8025(8) 0.112(7) Uiso 0.391(11) 1 d PDU A 2 C4' C 0.447(2) 0.2260(11) 0.8395(13) 0.111(7) Uiso 0.391(11) 1 d PDU A 2 F3Z F 0.553(3) 0.271(2) 0.7350(16) 0.096(6) Uiso 0.391(11) 1 d PDU A 2 F4Z F 0.5812(18) 0.220(2) 0.888(2) 0.133(7) Uiso 0.391(11) 1 d PDU A 2 F2Z F 0.650(2) 0.478(2) 0.9099(15) 0.075(5) Uiso 0.391(11) 1 d PDU A 2 F3Y F 0.334(3) 0.280(3) 0.745(2) 0.131(7) Uiso 0.391(11) 1 d PDU A 2 F4Y F 0.374(3) 0.270(2) 0.9110(18) 0.117(6) Uiso 0.391(11) 1 d PDU A 2 F2Y F 0.403(2) 0.488(2) 0.8803(17) 0.070(4) Uiso 0.391(11) 1 d PDU A 2 F4X F 0.357(3) 0.1091(13) 0.7972(17) 0.121(10) Uiso 0.391(11) 1 d PD A 2 O11B O 0.9325(13) 0.8327(10) 0.7372(9) 0.095(4) Uani 1 1 d . . . O11A O 0.6790(11) 0.7944(8) 0.6749(7) 0.066(2) Uani 1 1 d . B . C11 C 0.8154(15) 0.8634(9) 0.7191(9) 0.059(3) Uani 1 1 d D . . C12 C 0.8270(16) 0.9977(9) 0.7542(12) 0.069(4) Uiso 0.598(15) 1 d PDU B 1 F12B F 0.6860(17) 1.0162(14) 0.7681(13) 0.083(4) Uiso 0.598(15) 1 d PDU B 1 F12A F 0.937(2) 1.0643(15) 0.8379(12) 0.100(5) Uiso 0.598(15) 1 d PDU B 1 F13B F 0.914(3) 1.189(2) 0.7337(19) 0.130(6) Uiso 0.598(15) 1 d PDU B 1 F13A F 1.015(4) 1.080(6) 0.661(4) 0.35(3) Uiso 0.598(15) 1 d PD B 1 F14B F 0.641(3) 1.011(2) 0.624(2) 0.148(7) Uiso 0.598(15) 1 d PDU B 1 F14A F 0.761(2) 0.9084(16) 0.5355(13) 0.103(5) Uiso 0.598(15) 1 d PDU B 1 F14C F 0.864(5) 1.116(3) 0.571(3) 0.26(2) Uiso 0.598(15) 1 d PD B 1 C13 C 0.876(5) 1.068(2) 0.691(2) 0.164(11) Uiso 0.598(15) 1 d PDU B 1 C14 C 0.773(3) 1.0238(17) 0.588(2) 0.29(2) Uiso 0.598(15) 1 d PDU B 1 C12' C 0.842(2) 0.9991(9) 0.7463(15) 0.069(4) Uiso 0.402(15) 1 d PDU B 2 C13' C 0.897(2) 1.071(2) 0.6846(16) 0.164(11) Uiso 0.402(15) 1 d PDU B 2 C14' C 0.793(2) 1.0141(19) 0.5812(17) 0.29(2) Uiso 0.402(15) 1 d PDU B 2 F13Y F 0.848(5) 1.170(3) 0.715(3) 0.133(7) Uiso 0.402(15) 1 d PDU B 2 F14Y F 0.650(3) 1.034(3) 0.586(3) 0.143(8) Uiso 0.402(15) 1 d PDU B 2 F12Y F 0.741(3) 1.027(2) 0.8046(18) 0.088(5) Uiso 0.402(15) 1 d PDU B 2 F14Z F 0.874(4) 0.932(2) 0.565(2) 0.108(6) Uiso 0.402(15) 1 d PDU B 2 F12Z F 0.991(3) 1.058(2) 0.803(2) 0.097(6) Uiso 0.402(15) 1 d PDU B 2 F13Z F 1.027(2) 1.043(2) 0.6589(18) 0.085(7) Uiso 0.402(15) 1 d PD B 2 F14X F 0.852(3) 1.083(2) 0.5338(19) 0.079(7) Uiso 0.402(15) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0433(5) 0.0556(6) 0.0580(6) 0.0120(5) 0.0060(4) 0.0110(4) Ag2 0.0924(8) 0.0591(7) 0.0610(7) 0.0244(5) 0.0287(6) 0.0301(6) N21 0.047(5) 0.043(5) 0.052(6) 0.020(5) 0.004(4) 0.015(4) N24 0.029(4) 0.051(6) 0.045(5) 0.018(4) 0.008(4) 0.015(4) C23 0.032(5) 0.033(6) 0.045(7) 0.011(5) 0.001(4) 0.005(4) C22 0.039(5) 0.046(6) 0.044(7) 0.021(6) 0.002(5) 0.008(5) C26 0.036(5) 0.045(6) 0.046(7) 0.021(5) -0.002(5) 0.010(5) C25 0.035(5) 0.042(6) 0.046(7) 0.016(5) 0.005(5) 0.015(5) C29 0.055(7) 0.035(6) 0.073(9) 0.018(6) 0.008(6) 0.006(5) C28 0.049(7) 0.062(8) 0.059(8) 0.023(7) 0.012(6) 0.009(6) C27 0.076(8) 0.046(7) 0.055(8) 0.019(6) 0.027(7) 0.021(6) C30 0.071(8) 0.053(8) 0.064(9) 0.026(7) 0.026(7) 0.014(6) N31 0.023(4) 0.057(6) 0.045(5) 0.015(5) 0.004(4) 0.004(4) C37 0.031(6) 0.069(9) 0.079(10) 0.009(7) 0.007(6) 0.018(6) C36 0.025(5) 0.040(6) 0.040(6) 0.007(5) 0.004(4) 0.008(4) C40 0.050(7) 0.048(7) 0.061(8) 0.005(6) 0.004(6) 0.020(6) C32 0.038(5) 0.053(7) 0.029(6) 0.008(5) 0.003(4) 0.025(5) O1S 0.046(5) 0.082(7) 0.066(6) 0.029(5) 0.009(4) 0.001(4) C1S 0.096(13) 0.098(13) 0.093(13) 0.037(11) 0.010(10) 0.009(10) O1A 0.043(5) 0.079(6) 0.075(6) 0.035(5) 0.005(4) 0.018(4) O1B 0.041(5) 0.073(6) 0.066(6) 0.029(5) 0.005(4) 0.001(4) C1 0.053(7) 0.045(7) 0.064(9) 0.012(6) 0.024(7) 0.018(6) O11B 0.079(7) 0.109(9) 0.108(9) 0.041(7) 0.000(6) 0.058(7) O11A 0.068(6) 0.055(5) 0.075(6) 0.021(5) 0.015(5) 0.024(5) C11 0.055(8) 0.075(9) 0.057(8) 0.034(7) 0.013(6) 0.023(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N24 2.315(9) . ? Ag1 N31 2.328(8) . ? Ag1 O1S 2.379(9) . ? Ag1 O11B 2.469(9) 2_766 ? Ag2 N21 2.263(10) . ? Ag2 O11A 2.321(9) . ? Ag2 O1B 2.450(9) . ? N21 C26 1.337(13) . ? N21 C22 1.348(14) . ? N24 C25 1.336(14) . ? N24 C23 1.346(13) . ? C23 C22 1.379(16) . ? C23 C28 1.492(16) . ? C22 C27 1.516(15) . ? C26 C25 1.398(16) . ? C26 C30 1.491(16) . ? C25 C29 1.513(15) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? N31 C32 1.333(13) . ? N31 C36 1.341(12) . ? C37 C32 1.506(14) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C36 C32 1.372(14) 2_655 ? C36 C40 1.515(15) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? C32 C36 1.372(14) 2_655 ? O1S C1S 1.380(18) . ? O1S H1SO 0.7940 . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C1S H1S3 0.9700 . ? O1A C1 1.197(14) . ? O1B C1 1.243(14) . ? C1 C2' 1.5397(10) . ? C1 C2 1.5402(10) . ? F2B C2 1.3501(10) . ? F2A C2 1.3502(10) . ? C2 C3 1.5399(10) . ? F4A C4 1.3497(10) . ? F3B C3 1.3499(11) . ? F3A C3 1.3500(10) . ? F4B C4 1.3497(10) . ? F4C C4 1.3498(10) . ? C3 C4 1.5397(10) . ? C2' F2Y 1.3499(10) . ? C2' F2Z 1.3500(10) . ? C2' C3' 1.5406(10) . ? C3' F3Y 1.3503(11) . ? C3' F3Z 1.3504(10) . ? C3' C4' 1.5404(10) . ? C4' F4X 1.3495(11) . ? C4' F4Z 1.3498(10) . ? C4' F4Y 1.3499(10) . ? O11B C11 1.218(14) . ? O11B Ag1 2.469(9) 2_766 ? O11A C11 1.241(14) . ? C11 C12 1.5400(7) . ? C11 C12' 1.5400(8) . ? C12 F12A 1.3500(11) . ? C12 F12B 1.3500(10) . ? C12 C13 1.5400(11) . ? F13B C13 1.3502(11) . ? F13A C13 1.3501(11) . ? F14B C14 1.3500(11) . ? F14A C14 1.3500(10) . ? F14C C14 1.3501(11) . ? C13 C14 1.5400(11) . ? C12' F12Z 1.3500(11) . ? C12' F12Y 1.3501(10) . ? C12' C13' 1.5401(11) . ? C13' F13Z 1.3502(11) . ? C13' F13Y 1.3502(10) . ? C13' C14' 1.5400(10) . ? C14' F14X 1.3501(11) . ? C14' F14Y 1.3501(11) . ? C14' F14Z 1.3501(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N24 Ag1 N31 120.4(3) . . ? N24 Ag1 O1S 126.0(3) . . ? N31 Ag1 O1S 101.6(3) . . ? N24 Ag1 O11B 92.3(3) . 2_766 ? N31 Ag1 O11B 123.4(4) . 2_766 ? O1S Ag1 O11B 90.9(4) . 2_766 ? N21 Ag2 O11A 130.3(3) . . ? N21 Ag2 O1B 119.9(3) . . ? O11A Ag2 O1B 107.1(3) . . ? C26 N21 C22 118.6(10) . . ? C26 N21 Ag2 121.4(8) . . ? C22 N21 Ag2 119.9(7) . . ? C25 N24 C23 119.8(10) . . ? C25 N24 Ag1 118.7(7) . . ? C23 N24 Ag1 121.0(7) . . ? N24 C23 C22 119.6(10) . . ? N24 C23 C28 118.0(10) . . ? C22 C23 C28 122.4(10) . . ? N21 C22 C23 121.4(10) . . ? N21 C22 C27 116.6(10) . . ? C23 C22 C27 121.8(10) . . ? N21 C26 C25 120.5(10) . . ? N21 C26 C30 117.9(11) . . ? C25 C26 C30 121.6(10) . . ? N24 C25 C26 120.1(10) . . ? N24 C25 C29 117.3(10) . . ? C26 C25 C29 122.6(10) . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 N31 C36 118.0(8) . . ? C32 N31 Ag1 121.7(6) . . ? C36 N31 Ag1 120.1(7) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N31 C36 C32 120.7(9) . 2_655 ? N31 C36 C40 117.7(9) . . ? C32 C36 C40 121.6(9) 2_655 . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N31 C32 C36 121.3(9) . 2_655 ? N31 C32 C37 115.5(9) . . ? C36 C32 C37 123.1(10) 2_655 . ? C1S O1S Ag1 122.5(9) . . ? C1S O1S H1SO 109.3 . . ? Ag1 O1S H1SO 108.3 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C1 O1B Ag2 92.8(6) . . ? O1A C1 O1B 130.2(9) . . ? O1A C1 C2' 118.5(11) . . ? O1B C1 C2' 110.7(11) . . ? O1A C1 C2 114.9(10) . . ? O1B C1 C2 114.9(10) . . ? F2B C2 F2A 103.2(11) . . ? F2B C2 C3 108.6(11) . . ? F2A C2 C3 117.7(12) . . ? F2B C2 C1 109.4(11) . . ? F2A C2 C1 110.8(11) . . ? C3 C2 C1 106.9(9) . . ? F3B C3 F3A 121.1(16) . . ? F3B C3 C4 105.2(14) . . ? F3A C3 C4 100.8(12) . . ? F3B C3 C2 114.1(14) . . ? F3A C3 C2 106.7(13) . . ? C4 C3 C2 107.4(11) . . ? F4B C4 F4A 102.16(10) . . ? F4B C4 F4C 102.16(11) . . ? F4A C4 F4C 102.15(10) . . ? F4B C4 C3 118.4(13) . . ? F4A C4 C3 118.7(13) . . ? F4C C4 C3 110.9(14) . . ? F2Y C2' F2Z 110.8(16) . . ? F2Y C2' C1 122.2(15) . . ? F2Z C2' C1 117.5(15) . . ? F2Y C2' C3' 102.6(15) . . ? F2Z C2' C3' 91.0(14) . . ? C1 C2' C3' 106.3(9) . . ? F3Y C3' F3Z 95(2) . . ? F3Y C3' C4' 88.8(18) . . ? F3Z C3' C4' 92.6(15) . . ? F3Y C3' C2' 109(2) . . ? F3Z C3' C2' 120.4(16) . . ? C4' C3' C2' 139.34(18) . . ? F4X C4' F4Z 102.17(10) . . ? F4X C4' F4Y 102.17(11) . . ? F4Z C4' F4Y 102.13(10) . . ? F4X C4' C3' 132.8(14) . . ? F4Z C4' C3' 112.0(18) . . ? F4Y C4' C3' 101.5(15) . . ? C11 O11B Ag1 163.8(11) . 2_766 ? C11 O11A Ag2 107.8(7) . . ? O11B C11 O11A 125.7(10) . . ? O11B C11 C12 120.6(12) . . ? O11A C11 C12 113.8(10) . . ? O11B C11 C12' 117.2(13) . . ? O11A C11 C12' 117.0(11) . . ? F12A C12 F12B 107.3(14) . . ? F12A C12 C11 112.2(13) . . ? F12B C12 C11 112.3(12) . . ? F12A C12 C13 102.0(18) . . ? F12B C12 C13 102.5(18) . . ? C11 C12 C13 119.3(14) . . ? F13A C13 F13B 91(3) . . ? F13A C13 C14 93(3) . . ? F13B C13 C14 110(2) . . ? F13A C13 C12 124(4) . . ? F13B C13 C12 115(2) . . ? C14 C13 C12 118(2) . . ? F14A C14 F14B 102(2) . . ? F14A C14 F14C 122(3) . . ? F14B C14 F14C 132(3) . . ? F14A C14 C13 112(2) . . ? F14B C14 C13 89(3) . . ? F14C C14 C13 92(2) . . ? F12Z C12' F12Y 105(2) . . ? F12Z C12' C11 107.1(16) . . ? F12Y C12' C11 105.3(16) . . ? F12Z C12' C13' 84.7(17) . . ? F12Y C12' C13' 122.3(16) . . ? C11 C12' C13' 125.9(17) . . ? F13Z C13' F13Y 139(3) . . ? F13Z C13' C14' 95.0(17) . . ? F13Y C13' C14' 97(2) . . ? F13Z C13' C12' 105.6(19) . . ? F13Y C13' C12' 106(2) . . ? C14' C13' C12' 112.3(19) . . ? F14X C14' F14Y 101(2) . . ? F14X C14' F14Z 104(2) . . ? F14Y C14' F14Z 147(3) . . ? F14X C14' C13' 107.3(18) . . ? F14Y C14' C13' 107(2) . . ? F14Z C14' C13' 86.1(19) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.234 _refine_diff_density_min -1.266 _refine_diff_density_rms 0.168 data_ilb1321 _database_code_depnum_ccdc_archive 'CCDC 903745' #TrackingRef 'SCSC2_step0(start)_1-EtOH_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 Ag4 F28 N6 O10' _chemical_formula_weight 1784.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.88140(10) _cell_length_b 12.5043(2) _cell_length_c 15.3463(4) _cell_angle_alpha 110.1500(10) _cell_angle_beta 96.9020(10) _cell_angle_gamma 104.0520(10) _cell_volume 1512.73(5) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 5596 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.14 _exptl_crystal_description 'block from a needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 1.419 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6921 _exptl_absorpt_correction_T_max 0.7006 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12119 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.53 _reflns_number_total 5752 _reflns_number_gt 4704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+5.9550P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5752 _refine_ls_number_parameters 393 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.2133 _refine_ls_wR_factor_gt 0.2003 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag2 Ag 0.81977(8) 0.40654(6) 0.87496(4) 0.0648(2) Uani 1 1 d . . . Ag1 Ag 0.35038(6) 0.22067(5) 0.68728(4) 0.0520(2) Uani 1 1 d D . . N21 N 0.3203(6) 0.3407(5) 0.8320(4) 0.0424(12) Uani 1 1 d . C . N24 N 0.2456(6) 0.4788(5) 0.9945(4) 0.0437(12) Uani 1 1 d . . . C22 C 0.3638(6) 0.4609(6) 0.8608(4) 0.0423(14) Uani 1 1 d . . . C23 C 0.3262(7) 0.5297(6) 0.9432(4) 0.0425(14) Uani 1 1 d . C . C25 C 0.2021(7) 0.3577(6) 0.9654(5) 0.0448(14) Uani 1 1 d . C . C26 C 0.2418(7) 0.2890(6) 0.8833(5) 0.0444(14) Uani 1 1 d . . . C28 C 0.3672(10) 0.6630(6) 0.9755(6) 0.0559(18) Uani 1 1 d . . . H28A H 0.3331 0.6951 1.0342 0.084 Uiso 1 1 calc R C . H28B H 0.3136 0.6827 0.9269 0.084 Uiso 1 1 calc R . . H28C H 0.4815 0.6975 0.9862 0.084 Uiso 1 1 calc R . . C29 C 0.1114(10) 0.3039(7) 1.0248(6) 0.0611(19) Uani 1 1 d . . . H29A H 0.0655 0.3610 1.0639 0.092 Uiso 1 1 calc R C . H29B H 0.1832 0.2843 1.0653 0.092 Uiso 1 1 calc R . . H29C H 0.0270 0.2319 0.9833 0.092 Uiso 1 1 calc R . . C30 C 0.1982(9) 0.1558(6) 0.8489(6) 0.0584(19) Uani 1 1 d . C . H30A H 0.2535 0.1262 0.7993 0.088 Uiso 1 1 calc R . . H30B H 0.0842 0.1212 0.8235 0.088 Uiso 1 1 calc R . . H30C H 0.2288 0.1335 0.9014 0.088 Uiso 1 1 calc R . . C27 C 0.4488(9) 0.5150(7) 0.8015(6) 0.0567(18) Uani 1 1 d . C . H27A H 0.4983 0.4601 0.7632 0.085 Uiso 1 1 calc R . . H27B H 0.5300 0.5892 0.8425 0.085 Uiso 1 1 calc R . . H27C H 0.3737 0.5311 0.7601 0.085 Uiso 1 1 calc R . . N31 N 0.1309(5) 0.0840(4) 0.5677(3) 0.0364(11) Uani 1 1 d . C . C32 C -0.0103(6) 0.1047(5) 0.5604(4) 0.0366(12) Uani 1 1 d . . . C37 C -0.0196(8) 0.2211(6) 0.6283(5) 0.0502(16) Uani 1 1 d . C . H37A H -0.0520 0.2107 0.6837 0.075 Uiso 1 1 calc R . . H37B H -0.0969 0.2470 0.5971 0.075 Uiso 1 1 calc R . . H37C H 0.0840 0.2809 0.6479 0.075 Uiso 1 1 calc R . . C36 C 0.1421(6) -0.0196(5) 0.5071(4) 0.0371(12) Uani 1 1 d . . . C40 C 0.3032(7) -0.0383(7) 0.5166(6) 0.058(2) Uani 1 1 d . C . H40A H 0.2923 -0.1181 0.5149 0.087 Uiso 1 1 calc R . . H40B H 0.3720 0.0203 0.5766 0.087 Uiso 1 1 calc R . . H40C H 0.3493 -0.0290 0.4645 0.087 Uiso 1 1 calc R . . O1A O 0.5695(9) 0.1749(8) 0.7706(5) 0.096(2) Uani 1 1 d . A . O1B O 0.8239(7) 0.2100(5) 0.8279(4) 0.0662(14) Uani 1 1 d . A . C1 C 0.6870(8) 0.1450(5) 0.7869(5) 0.0519(16) Uiso 1 1 d D . . C3 C 0.5986(14) -0.0613(12) 0.8137(8) 0.34(2) Uiso 0.484(11) 1 d PDU A 1 C2 C 0.6609(12) 0.0095(5) 0.7541(6) 0.062(2) Uiso 0.484(11) 1 d PDU A 1 F2A F 0.5120(10) -0.0530(12) 0.7011(10) 0.092(3) Uiso 0.484(11) 1 d PDU A 1 F2B F 0.7606(13) -0.0203(11) 0.6966(9) 0.085(3) Uiso 0.484(11) 1 d PDU A 1 F3A F 0.569(2) -0.1811(13) 0.7817(14) 0.131(5) Uiso 0.484(11) 1 d PDU A 1 F3B F 0.472(3) -0.0384(17) 0.848(2) 0.193(7) Uiso 0.484(11) 1 d PDU A 1 F4B F 0.8453(18) -0.0458(14) 0.8961(15) 0.179(7) Uiso 0.484(11) 1 d PDU A 1 C4 C 0.7074(13) -0.0238(10) 0.9120(8) 0.44(3) Uiso 0.484(11) 1 d PDU A 1 F4A F 0.745(2) 0.0952(11) 0.9615(11) 0.115(4) Uiso 0.484(11) 1 d PDU A 1 F4C F 0.6400(14) -0.0993(11) 0.9515(9) 0.091(4) Uiso 0.484(11) 1 d PD A 1 F3Z F 0.6412(18) -0.1799(13) 0.7735(12) 0.107(4) Uiso 0.516(11) 1 d PDU A 2 F4Z F 0.6486(19) 0.0738(14) 0.9390(12) 0.125(4) Uiso 0.516(11) 1 d PDU A 2 F2Z F 0.5586(12) -0.0564(12) 0.6736(8) 0.092(3) Uiso 0.516(11) 1 d PDU A 2 F2Y F 0.8075(10) -0.0115(10) 0.7378(9) 0.078(3) Uiso 0.516(11) 1 d PDU A 2 F4Y F 0.8329(19) 0.0079(18) 0.8803(15) 0.165(6) Uiso 0.516(11) 1 d PDU A 2 F4X F 0.664(5) -0.1417(14) 0.891(4) 0.41(3) Uiso 0.516(11) 1 d PD A 2 F3Y F 0.488(3) -0.0869(16) 0.845(2) 0.223(8) Uiso 0.516(11) 1 d PDU A 2 C2' C 0.6703(11) 0.0109(5) 0.7549(7) 0.062(2) Uiso 0.516(11) 1 d PDU A 2 C3' C 0.617(2) -0.0718(9) 0.8076(10) 0.34(2) Uiso 0.516(11) 1 d PDU A 2 C4' C 0.702(2) -0.0226(13) 0.9134(10) 0.44(3) Uiso 0.516(11) 1 d PDU A 2 O11A O 0.7901(6) 0.4528(5) 0.7290(4) 0.0648(14) Uani 1 1 d . B . O11B O 1.0381(7) 0.4989(6) 0.8049(4) 0.0672(14) Uani 1 1 d . B . C11 C 0.9370(8) 0.4961(6) 0.7423(4) 0.0499(15) Uiso 1 1 d D . . C12 C 0.9887(13) 0.5504(7) 0.6704(5) 0.056(2) Uiso 0.421(9) 1 d PDU B 1 F12A F 0.8749(12) 0.5244(14) 0.5931(8) 0.078(3) Uiso 0.421(9) 1 d PDU B 1 C13 C 1.0415(13) 0.6876(7) 0.7211(4) 0.082(4) Uiso 0.421(9) 1 d PDU B 1 F14B F 1.1550(17) 0.8723(6) 0.7098(9) 0.114(5) Uiso 0.421(9) 1 d PDU B 1 F13A F 1.1743(13) 0.7292(14) 0.7908(9) 0.101(5) Uiso 0.421(9) 1 d PD B 1 F14A F 0.9332(13) 0.7569(13) 0.6107(12) 0.144(5) Uiso 0.421(9) 1 d PDU B 1 F13B F 0.9295(15) 0.7277(14) 0.7626(10) 0.099(4) Uiso 0.421(9) 1 d PDU B 1 F14C F 1.1676(18) 0.7132(10) 0.5996(9) 0.127(6) Uiso 0.421(9) 1 d PD B 1 C14 C 1.0731(10) 0.7567(6) 0.6560(6) 0.100(4) Uiso 0.421(9) 1 d PDU B 1 F12B F 1.1104(14) 0.5145(13) 0.6384(9) 0.071(3) Uiso 0.421(9) 1 d PDU B 1 C14' C 1.0809(8) 0.7540(5) 0.6505(5) 0.101(4) Uiso 0.579(9) 1 d PDU B 2 C13' C 1.0080(10) 0.6864(6) 0.7099(5) 0.083(3) Uiso 0.579(9) 1 d PDU B 2 C12' C 0.9998(10) 0.5535(6) 0.6744(5) 0.055(2) Uiso 0.579(9) 1 d PDU B 2 F13Z F 1.0878(13) 0.7448(11) 0.8017(6) 0.117(4) Uiso 0.579(9) 1 d PD B 2 F14Z F 0.9917(14) 0.7031(9) 0.5607(5) 0.127(4) Uiso 0.579(9) 1 d PDU B 2 F12Z F 0.9049(10) 0.4911(10) 0.5865(6) 0.080(3) Uiso 0.579(9) 1 d PDU B 2 F12Y F 1.1472(9) 0.5469(10) 0.6663(7) 0.079(3) Uiso 0.579(9) 1 d PDU B 2 F13Y F 0.8568(10) 0.6896(10) 0.7082(8) 0.098(3) Uiso 0.579(9) 1 d PDU B 2 F14Y F 1.0749(15) 0.8673(5) 0.6861(8) 0.136(4) Uiso 0.579(9) 1 d PDU B 2 F14X F 1.2365(9) 0.7616(11) 0.6591(10) 0.148(6) Uiso 0.579(9) 1 d PD B 2 O1S O 0.5308(15) 0.2929(16) 0.6027(10) 0.067(5) Uiso 0.56(4) 1 d PD C 1 H1S H 0.6366 0.2953 0.6219 0.100 Uiso 0.56(4) 1 calc PR C 1 C1S C 0.506(6) 0.329(4) 0.534(2) 0.20(2) Uiso 0.56(4) 1 d PD C 1 H1S1 H 0.5605 0.4157 0.5586 0.237 Uiso 0.56(4) 1 calc PR C 1 H1S2 H 0.5566 0.2906 0.4838 0.237 Uiso 0.56(4) 1 calc PR C 1 C2S C 0.367(3) 0.312(3) 0.497(2) 0.135(12) Uiso 0.56(4) 1 d PD C 1 H2S1 H 0.2975 0.2559 0.5166 0.202 Uiso 0.56(4) 1 calc PR C 1 H2S2 H 0.3521 0.2791 0.4285 0.202 Uiso 0.56(4) 1 calc PR C 1 H2S3 H 0.3425 0.3870 0.5175 0.202 Uiso 0.56(4) 1 calc PR C 1 O1S' O 0.5417(14) 0.2673(16) 0.5991(9) 0.044(4) Uiso 0.44(4) 1 d PD C 2 H1S' H 0.6478 0.2702 0.6182 0.066 Uiso 0.44(4) 1 calc PR C 2 C1S' C 0.494(3) 0.291(3) 0.5171(15) 0.068(7) Uiso 0.44(4) 1 d PD C 2 H1S3 H 0.4154 0.2184 0.4691 0.082 Uiso 0.44(4) 1 calc PR C 2 H1S4 H 0.5870 0.3093 0.4901 0.082 Uiso 0.44(4) 1 calc PR C 2 C2S' C 0.423(4) 0.395(3) 0.540(2) 0.102(11) Uiso 0.44(4) 1 d PD C 2 H2S4 H 0.3201 0.3717 0.5550 0.153 Uiso 0.44(4) 1 calc PR C 2 H2S5 H 0.4086 0.4162 0.4844 0.153 Uiso 0.44(4) 1 calc PR C 2 H2S6 H 0.4938 0.4641 0.5932 0.153 Uiso 0.44(4) 1 calc PR C 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 Ag2 0.0889(5) 0.0551(4) 0.0521(4) 0.0147(3) 0.0261(3) 0.0288(3) Ag1 0.0420(3) 0.0521(3) 0.0448(3) 0.0020(2) 0.0028(2) 0.0126(2) N21 0.032(2) 0.041(3) 0.041(3) 0.004(2) 0.0005(19) 0.0099(19) N24 0.042(3) 0.045(3) 0.035(3) 0.007(2) 0.003(2) 0.012(2) C22 0.030(3) 0.043(3) 0.039(3) 0.004(3) -0.002(2) 0.007(2) C23 0.040(3) 0.039(3) 0.038(3) 0.006(3) -0.003(2) 0.012(2) C25 0.041(3) 0.043(3) 0.042(3) 0.009(3) 0.003(2) 0.012(3) C26 0.035(3) 0.043(3) 0.044(3) 0.007(3) -0.001(2) 0.010(2) C28 0.070(4) 0.040(4) 0.052(4) 0.011(3) 0.014(3) 0.016(3) C29 0.071(5) 0.048(4) 0.057(4) 0.016(3) 0.017(4) 0.012(3) C30 0.057(4) 0.041(4) 0.066(5) 0.009(3) 0.014(3) 0.012(3) C27 0.056(4) 0.049(4) 0.058(4) 0.014(3) 0.020(3) 0.011(3) N31 0.028(2) 0.037(2) 0.035(2) 0.006(2) 0.0037(17) 0.0080(18) C32 0.031(2) 0.035(3) 0.037(3) 0.008(2) 0.007(2) 0.009(2) C37 0.043(3) 0.045(4) 0.051(4) 0.003(3) 0.006(3) 0.019(3) C36 0.028(2) 0.039(3) 0.039(3) 0.008(2) 0.007(2) 0.012(2) C40 0.032(3) 0.055(4) 0.067(5) 0.001(3) -0.001(3) 0.018(3) O1A 0.088(5) 0.115(6) 0.093(5) 0.035(4) 0.003(4) 0.062(4) O1B 0.061(3) 0.054(3) 0.073(4) 0.011(3) 0.013(3) 0.019(2) O11A 0.045(3) 0.071(3) 0.058(3) 0.014(3) 0.006(2) 0.002(2) O11B 0.058(3) 0.075(4) 0.065(3) 0.028(3) 0.005(3) 0.019(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 Ag2 N24 2.261(5) 2_667 ? Ag2 O1B 2.321(6) . ? Ag2 O11A 2.499(6) . ? Ag2 O11B 2.554(6) . ? Ag1 N21 2.302(5) . ? Ag1 N31 2.334(4) . ? Ag1 O1S' 2.382(5) . ? Ag1 O1S 2.382(5) . ? Ag1 O1A 2.489(6) . ? N21 C26 1.336(9) . ? N21 C22 1.351(8) . ? N24 C23 1.341(9) . ? N24 C25 1.360(9) . ? N24 Ag2 2.261(5) 2_667 ? C22 C23 1.394(9) . ? C22 C27 1.482(10) . ? C23 C28 1.500(10) . ? C25 C26 1.399(9) . ? C25 C29 1.505(11) . ? C26 C30 1.496(10) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? N31 C32 1.341(7) . ? N31 C36 1.345(7) . ? C32 C36 1.386(8) 2_556 ? C32 C37 1.498(8) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C36 C32 1.386(8) 2_556 ? C36 C40 1.503(8) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? O1A C1 1.218(9) . ? O1B C1 1.233(9) . ? C1 C2 1.5399(10) . ? C1 C2' 1.5402(10) . ? C3 F3B 1.3501(10) . ? C3 F3A 1.3501(10) . ? C3 C4 1.5399(10) . ? C3 C2 1.5400(10) . ? C2 F2A 1.3500(10) . ? C2 F2B 1.3500(10) . ? F4B C4 1.3499(10) . ? C4 F4A 1.3499(11) . ? C4 F4C 1.3499(10) . ? F3Z C3' 1.3502(11) . ? F4Z C4' 1.3499(10) . ? F2Z C2' 1.3502(10) . ? F2Y C2' 1.3502(10) . ? F4Y C4' 1.3499(11) . ? F4X C4' 1.3499(11) . ? F3Y C3' 1.3503(10) . ? C2' C3' 1.5402(10) . ? C3' C4' 1.5400(10) . ? O11A C11 1.247(8) . ? O11B C11 1.218(9) . ? C11 C12' 1.5397(10) . ? C11 C12 1.5406(10) . ? C12 F12A 1.3503(10) . ? C12 F12B 1.3503(10) . ? C12 C13 1.5397(10) . ? C13 F13A 1.3499(10) . ? C13 F13B 1.3499(10) . ? C13 C14 1.5392(10) . ? F14B C14 1.3501(11) . ? F14A C14 1.3496(10) . ? F14C C14 1.3495(10) . ? C14' F14Y 1.3492(10) . ? C14' F14Z 1.3492(10) . ? C14' F14X 1.3494(10) . ? C14' C13' 1.5395(10) . ? C13' F13Y 1.3500(10) . ? C13' F13Z 1.3500(10) . ? C13' C12' 1.5400(10) . ? C12' F12Y 1.3500(10) . ? C12' F12Z 1.3501(10) . ? O1S C1S 1.30(2) . ? O1S H1S 0.9400 . ? C1S C2S 1.22(4) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C2S H2S3 0.9700 . ? O1S' C1S' 1.43(2) . ? O1S' H1S' 0.9400 . ? C1S' C2S' 1.55(4) . ? C1S' H1S3 0.9800 . ? C1S' H1S4 0.9800 . ? C2S' H2S4 0.9700 . ? C2S' H2S5 0.9700 . ? C2S' H2S6 0.9700 . ? 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 N24 Ag2 O1B 129.8(2) 2_667 . ? N24 Ag2 O11A 118.7(2) 2_667 . ? O1B Ag2 O11A 107.5(2) . . ? N24 Ag2 O11B 120.7(2) 2_667 . ? O1B Ag2 O11B 102.6(2) . . ? O11A Ag2 O11B 51.63(17) . . ? N21 Ag1 N31 121.43(16) . . ? N21 Ag1 O1S' 128.5(4) . . ? N31 Ag1 O1S' 102.6(4) . . ? N21 Ag1 O1S 122.8(5) . . ? N31 Ag1 O1S 103.9(4) . . ? O1S' Ag1 O1S 8.3(6) . . ? N21 Ag1 O1A 89.9(2) . . ? N31 Ag1 O1A 127.1(2) . . ? O1S' Ag1 O1A 82.9(5) . . ? O1S Ag1 O1A 88.6(5) . . ? C26 N21 C22 119.4(5) . . ? C26 N21 Ag1 118.7(4) . . ? C22 N21 Ag1 121.4(4) . . ? C23 N24 C25 118.8(5) . . ? C23 N24 Ag2 120.0(4) . 2_667 ? C25 N24 Ag2 121.2(4) . 2_667 ? N21 C22 C23 119.8(6) . . ? N21 C22 C27 118.0(6) . . ? C23 C22 C27 122.2(6) . . ? N24 C23 C22 121.2(6) . . ? N24 C23 C28 117.3(6) . . ? C22 C23 C28 121.4(6) . . ? N24 C25 C26 119.8(6) . . ? N24 C25 C29 117.2(6) . . ? C26 C25 C29 123.0(6) . . ? N21 C26 C25 120.9(6) . . ? N21 C26 C30 117.2(6) . . ? C25 C26 C30 121.9(7) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C32 N31 C36 118.6(5) . . ? C32 N31 Ag1 120.9(4) . . ? C36 N31 Ag1 120.5(4) . . ? N31 C32 C36 120.3(5) . 2_556 ? N31 C32 C37 117.6(5) . . ? C36 C32 C37 122.1(5) 2_556 . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N31 C36 C32 121.1(5) . 2_556 ? N31 C36 C40 116.8(5) . . ? C32 C36 C40 122.0(5) 2_556 . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1 O1A Ag1 161.9(7) . . ? C1 O1B Ag2 107.3(4) . . ? O1A C1 O1B 127.9(7) . . ? O1A C1 C2 116.1(7) . . ? O1B C1 C2 115.9(6) . . ? O1A C1 C2' 119.0(7) . . ? O1B C1 C2' 113.1(7) . . ? F3B C3 F3A 106.28(11) . . ? F3B C3 C4 94.9(17) . . ? F3A C3 C4 99.8(13) . . ? F3B C3 C2 115.1(17) . . ? F3A C3 C2 121.4(13) . . ? C4 C3 C2 115.17(11) . . ? F2A C2 F2B 106.27(11) . . ? F2A C2 C1 110.8(9) . . ? F2B C2 C1 108.6(8) . . ? F2A C2 C3 79.4(8) . . ? F2B C2 C3 123.0(10) . . ? C1 C2 C3 122.2(8) . . ? F4A C4 F4C 119.0(12) . . ? F4A C4 F4B 106.27(11) . . ? F4C C4 F4B 106.29(11) . . ? F4A C4 C3 110.7(10) . . ? F4C C4 C3 107.2(9) . . ? F4B C4 C3 106.7(14) . . ? F2Z C2' F2Y 106.22(11) . . ? F2Z C2' C1 112.4(9) . . ? F2Y C2' C1 111.8(8) . . ? F2Z C2' C3' 95.6(9) . . ? F2Y C2' C3' 100.3(10) . . ? C1 C2' C3' 127.9(7) . . ? F3Z C3' F3Y 106.24(11) . . ? F3Z C3' C4' 102.1(14) . . ? F3Y C3' C4' 80.9(18) . . ? F3Z C3' C2' 116.1(12) . . ? F3Y C3' C2' 128.6(18) . . ? C4' C3' C2' 115.15(11) . . ? F4Z C4' F4X 145.7(11) . . ? F4Z C4' F4Y 106.30(11) . . ? F4X C4' F4Y 106.28(11) . . ? F4Z C4' C3' 94.9(12) . . ? F4X C4' C3' 79(3) . . ? F4Y C4' C3' 83.1(12) . . ? C11 O11A Ag2 91.8(4) . . ? C11 O11B Ag2 89.9(4) . . ? O11B C11 O11A 126.5(5) . . ? O11B C11 C12' 115.7(6) . . ? O11A C11 C12' 117.8(6) . . ? O11B C11 C12 119.4(7) . . ? O11A C11 C12 114.1(7) . . ? F12A C12 F12B 106.93(11) . . ? F12A C12 C13 105.2(8) . . ? F12B C12 C13 109.9(10) . . ? F12A C12 C11 116.1(9) . . ? F12B C12 C11 110.3(9) . . ? C13 C12 C11 108.3(6) . . ? F13A C13 F13B 106.27(11) . . ? F13A C13 C14 106.9(9) . . ? F13B C13 C14 102.9(9) . . ? F13A C13 C12 112.2(10) . . ? F13B C13 C12 112.4(10) . . ? C14 C13 C12 115.28(11) . . ? F14C C14 F14A 115.9(3) . . ? F14C C14 F14B 106.28(11) . . ? F14A C14 F14B 106.28(11) . . ? F14C C14 C13 109.41(11) . . ? F14A C14 C13 109.41(11) . . ? F14B C14 C13 109.36(11) . . ? F14Y C14' F14Z 106.37(11) . . ? F14Y C14' F14X 106.37(11) . . ? F14Z C14' F14X 115.7(3) . . ? F14Y C14' C13' 109.40(11) . . ? F14Z C14' C13' 109.39(11) . . ? F14X C14' C13' 109.39(11) . . ? F13Y C13' F13Z 106.27(11) . . ? F13Y C13' C14' 108.8(7) . . ? F13Z C13' C14' 109.2(7) . . ? F13Y C13' C12' 106.5(8) . . ? F13Z C13' C12' 110.5(8) . . ? C14' C13' C12' 115.18(11) . . ? F12Y C12' F12Z 106.27(11) . . ? F12Y C12' C11 111.4(7) . . ? F12Z C12' C11 108.7(7) . . ? F12Y C12' C13' 107.8(7) . . ? F12Z C12' C13' 111.2(7) . . ? C11 C12' C13' 111.4(5) . . ? C1S O1S Ag1 130(3) . . ? C1S O1S H1S 114.9 . . ? Ag1 O1S H1S 114.9 . . ? C2S C1S O1S 117(4) . . ? C2S C1S H1S1 108.0 . . ? O1S C1S H1S1 108.0 . . ? C2S C1S H1S2 108.0 . . ? O1S C1S H1S2 108.0 . . ? H1S1 C1S H1S2 107.3 . . ? C1S' O1S' Ag1 119.5(12) . . ? C1S' O1S' H1S' 120.2 . . ? Ag1 O1S' H1S' 120.2 . . ? O1S' C1S' C2S' 113(2) . . ? O1S' C1S' H1S3 109.0 . . ? C2S' C1S' H1S3 109.0 . . ? O1S' C1S' H1S4 109.0 . . ? C2S' C1S' H1S4 109.0 . . ? H1S3 C1S' H1S4 107.8 . . ? C1S' C2S' H2S4 109.5 . . ? C1S' C2S' H2S5 109.5 . . ? H2S4 C2S' H2S5 109.5 . . ? C1S' C2S' H2S6 109.5 . . ? H2S4 C2S' H2S6 109.5 . . ? H2S5 C2S' H2S6 109.5 . . ? _diffrn_measured_fraction_theta_max 0.825 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.825 _refine_diff_density_max 1.600 _refine_diff_density_min -1.459 _refine_diff_density_rms 0.146 data_ilb1333_0m _database_code_depnum_ccdc_archive 'CCDC 903746' #TrackingRef 'SCSC2_step1_1_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 Ag4 F28 N6 O8' _chemical_formula_weight 1692.22 _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5215(2) _cell_length_b 12.9026(3) _cell_length_c 14.8408(4) _cell_angle_alpha 67.1460(10) _cell_angle_beta 89.5140(10) _cell_angle_gamma 70.6750(10) _cell_volume 1405.34(6) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.12 _exptl_crystal_description 'block from a needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.519 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6758 _exptl_absorpt_correction_T_max 0.6846 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25544 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6404 _reflns_number_gt 3951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+8.8900P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6404 _refine_ls_number_parameters 376 _refine_ls_number_restraints 295 _refine_ls_R_factor_all 0.1214 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.2465 _refine_ls_wR_factor_gt 0.1945 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.14327(9) -0.07095(7) 1.29208(6) 0.0608(3) Uani 1 1 d . . . Ag2 Ag 0.59207(10) 0.01542(7) 0.87654(5) 0.0630(3) Uani 1 1 d . . . N21 N 0.7498(8) -0.0138(6) 1.0131(5) 0.0436(11) Uani 1 1 d U . . C22 C 0.8492(10) -0.1209(7) 1.0720(6) 0.0441(12) Uani 1 1 d U . . C23 C 0.9550(10) -0.1374(7) 1.1514(6) 0.0452(12) Uani 1 1 d U . . N24 N 0.9558(8) -0.0429(6) 1.1678(5) 0.0454(12) Uani 1 1 d U . . C25 C 0.8506(10) 0.0667(7) 1.1089(6) 0.0465(13) Uani 1 1 d U . . C26 C 0.7472(11) 0.0825(7) 1.0295(6) 0.0478(13) Uani 1 1 d U . . C27 C 0.8412(12) -0.2261(8) 1.0547(7) 0.0551(19) Uani 1 1 d U . . H27A H 0.7642 -0.1974 0.9953 0.083 Uiso 1 1 calc R . . H27B H 0.8022 -0.2765 1.1106 0.083 Uiso 1 1 calc R . . H27C H 0.9521 -0.2725 1.0471 0.083 Uiso 1 1 calc R . . C28 C 1.0673(12) -0.2603(8) 1.2228(7) 0.058(2) Uani 1 1 d U . . H28A H 1.1446 -0.2523 1.2651 0.086 Uiso 1 1 calc R . . H28B H 1.1303 -0.3048 1.1864 0.086 Uiso 1 1 calc R . . H28C H 0.9995 -0.3030 1.2628 0.086 Uiso 1 1 calc R . . C29 C 0.8457(12) 0.1690(8) 1.1353(7) 0.0581(19) Uani 1 1 d U . . H29A H 0.7355 0.2030 1.1517 0.087 Uiso 1 1 calc R . . H29B H 0.8685 0.2304 1.0795 0.087 Uiso 1 1 calc R . . H29C H 0.9300 0.1395 1.1916 0.087 Uiso 1 1 calc R . . C30 C 0.6301(13) 0.2053(8) 0.9604(7) 0.061(2) Uani 1 1 d U . . H30A H 0.6925 0.2593 0.9367 0.091 Uiso 1 1 calc R . . H30B H 0.5423 0.2363 0.9951 0.091 Uiso 1 1 calc R . . H30C H 0.5802 0.1996 0.9048 0.091 Uiso 1 1 calc R . . N31 N 1.0601(8) -0.0509(6) 1.4350(5) 0.0449(12) Uani 1 1 d U . . C36 C 0.8985(10) -0.0240(8) 1.4482(6) 0.0468(14) Uani 1 1 d U . . C32 C 1.1619(9) -0.0291(8) 1.4867(6) 0.0446(14) Uani 1 1 d U . . C37 C 1.3467(10) -0.0676(9) 1.4742(7) 0.0557(19) Uani 1 1 d U . . H37A H 1.3666 -0.1116 1.4325 0.084 Uiso 1 1 calc R . . H37B H 1.4140 -0.1187 1.5383 0.084 Uiso 1 1 calc R . . H37C H 1.3774 0.0032 1.4436 0.084 Uiso 1 1 calc R . . C40 C 0.7889(11) -0.0564(9) 1.3922(7) 0.0548(18) Uani 1 1 d U . . H40A H 0.8591 -0.1115 1.3662 0.082 Uiso 1 1 calc R . . H40B H 0.7165 0.0159 1.3382 0.082 Uiso 1 1 calc R . . H40C H 0.7207 -0.0945 1.4364 0.082 Uiso 1 1 calc R . . O11B O 0.3860(11) 0.1837(8) 0.7640(7) 0.0896(19) Uani 1 1 d U A . O11A O 0.5971(11) 0.2175(8) 0.6896(7) 0.0909(19) Uani 1 1 d U . . C11 C 0.4494(15) 0.2436(8) 0.6993(8) 0.0885(16) Uani 1 1 d DU . . F13Z F 0.4689(14) 0.4752(15) 0.6800(11) 0.118(3) Uiso 0.558(8) 1 d PDU A 1 F14Y F 0.2486(16) 0.6323(9) 0.5036(6) 0.129(3) Uiso 0.558(8) 1 d PDU A 1 F13Y F 0.2512(17) 0.4420(14) 0.7422(10) 0.107(3) Uiso 0.558(8) 1 d PDU A 1 F12Z F 0.1830(14) 0.3524(13) 0.6031(10) 0.092(3) Uiso 0.558(8) 1 d PDU A 1 F12Y F 0.3834(16) 0.4110(14) 0.5387(10) 0.102(3) Uiso 0.558(8) 1 d PDU A 1 C14' C 0.1967(10) 0.5923(6) 0.5927(6) 0.118(2) Uiso 0.558(8) 1 d PDU A 1 C12' C 0.3263(13) 0.3658(6) 0.6253(7) 0.0948(17) Uiso 0.558(8) 1 d PDU A 1 C13' C 0.3218(12) 0.4661(7) 0.6582(6) 0.1076(18) Uiso 0.558(8) 1 d PDU A 1 F14Z F 0.0461(9) 0.5849(9) 0.5761(11) 0.130(3) Uiso 0.558(8) 1 d PDU A 1 F14X F 0.1977(18) 0.6699(9) 0.6327(10) 0.129(3) Uiso 0.558(8) 1 d PDU A 1 F12B F 0.1695(17) 0.3830(16) 0.6257(12) 0.088(3) Uiso 0.442(8) 1 d PDU A 2 F12A F 0.364(2) 0.3656(18) 0.5326(11) 0.100(3) Uiso 0.442(8) 1 d PDU A 2 F13B F 0.348(2) 0.4397(18) 0.7496(8) 0.109(3) Uiso 0.442(8) 1 d PDU A 2 F13A F 0.4825(19) 0.4749(18) 0.6235(12) 0.107(3) Uiso 0.442(8) 1 d PDU A 2 F14B F 0.1801(19) 0.5963(8) 0.4933(7) 0.129(3) Uiso 0.442(8) 1 d PDU A 2 C14 C 0.2153(12) 0.5949(7) 0.5824(7) 0.118(2) Uiso 0.442(8) 1 d PDU A 2 F14A F 0.0677(15) 0.6207(14) 0.6181(12) 0.129(3) Uiso 0.442(8) 1 d PDU A 2 F14C F 0.295(2) 0.6739(11) 0.5670(14) 0.134(3) Uiso 0.442(8) 1 d PDU A 2 C12 C 0.3339(15) 0.3663(6) 0.6218(8) 0.0950(17) Uiso 0.442(8) 1 d PDU A 2 C13 C 0.3338(14) 0.4681(9) 0.6517(7) 0.1076(18) Uiso 0.442(8) 1 d PDU A 2 O1A O 0.5447(10) -0.1317(7) 0.8307(6) 0.0795(16) Uani 1 1 d U B . O1B O 0.7733(11) -0.1115(8) 0.7728(7) 0.0855(17) Uani 1 1 d U . . C1 C 0.6613(17) -0.1558(9) 0.7881(9) 0.0816(15) Uani 1 1 d DU . . F4Z F 0.5544(13) -0.4153(13) 0.9053(11) 0.117(3) Uiso 0.654(8) 1 d PDU B 1 F4X F 0.8258(16) -0.5512(7) 0.9599(9) 0.109(3) Uiso 0.654(8) 1 d PDU B 1 F4Y F 0.7446(16) -0.3803(9) 0.9718(10) 0.111(3) Uiso 0.654(8) 1 d PDU B 1 F2Z F 0.7208(13) -0.2294(11) 0.6615(7) 0.093(2) Uiso 0.654(8) 1 d PDU B 1 F3Y F 0.7607(15) -0.4522(11) 0.7633(10) 0.108(3) Uiso 0.654(8) 1 d PDU B 1 C2' C 0.6590(11) -0.2492(7) 0.7483(5) 0.0894(16) Uiso 0.654(8) 1 d PDU B 1 C3' C 0.7651(11) -0.3822(8) 0.8105(7) 0.0985(18) Uiso 0.654(8) 1 d PDU B 1 C4' C 0.7205(12) -0.4357(8) 0.9153(6) 0.103(2) Uiso 0.654(8) 1 d PDU B 1 F2Y F 0.5029(11) -0.2482(10) 0.7318(7) 0.081(2) Uiso 0.654(8) 1 d PDU B 1 F3Z F 0.9285(14) -0.3988(12) 0.8290(11) 0.112(3) Uiso 0.654(8) 1 d PDU B 1 C2 C 0.6984(18) -0.2498(8) 0.7436(7) 0.0898(17) Uiso 0.346(8) 1 d PDU B 2 C3 C 0.7990(12) -0.3775(11) 0.8204(11) 0.0988(18) Uiso 0.346(8) 1 d PDU B 2 C4 C 0.6980(19) -0.4370(12) 0.8973(10) 0.104(2) Uiso 0.346(8) 1 d PDU B 2 F4A F 0.559(3) -0.440(3) 0.857(2) 0.126(4) Uiso 0.346(8) 1 d PDU B 2 F4C F 0.743(3) -0.5565(11) 0.9514(15) 0.107(4) Uiso 0.346(8) 1 d PDU B 2 F3A F 0.927(2) -0.383(2) 0.8776(18) 0.108(4) Uiso 0.346(8) 1 d PDU B 2 F2A F 0.5559(18) -0.2392(19) 0.6960(14) 0.088(3) Uiso 0.346(8) 1 d PDU B 2 F2B F 0.806(2) -0.236(2) 0.6764(13) 0.094(3) Uiso 0.346(8) 1 d PDU B 2 F3B F 0.866(3) -0.4591(19) 0.7820(17) 0.106(3) Uiso 0.346(8) 1 d PDU B 2 F4B F 0.647(3) -0.3839(16) 0.9603(16) 0.110(3) Uiso 0.346(8) 1 d PDU B 2 _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 0.0504(4) 0.0780(5) 0.0631(5) -0.0414(4) 0.0046(3) -0.0188(3) Ag2 0.0662(5) 0.0667(5) 0.0547(4) -0.0267(4) -0.0011(3) -0.0192(4) N21 0.047(2) 0.045(2) 0.043(2) -0.0204(19) 0.0060(19) -0.0173(19) C22 0.048(2) 0.044(2) 0.045(2) -0.0215(19) 0.007(2) -0.0180(19) C23 0.046(2) 0.045(2) 0.047(2) -0.020(2) 0.010(2) -0.017(2) N24 0.045(2) 0.046(2) 0.047(2) -0.0194(19) 0.012(2) -0.0185(19) C25 0.048(2) 0.045(2) 0.050(2) -0.020(2) 0.010(2) -0.019(2) C26 0.048(2) 0.046(2) 0.047(2) -0.018(2) 0.010(2) -0.016(2) C27 0.063(4) 0.048(4) 0.055(4) -0.027(3) 0.000(3) -0.014(3) C28 0.056(4) 0.050(4) 0.059(4) -0.018(3) 0.001(3) -0.014(3) C29 0.058(4) 0.049(4) 0.065(4) -0.024(3) 0.000(4) -0.014(3) C30 0.065(4) 0.047(4) 0.056(4) -0.013(3) -0.001(4) -0.011(3) N31 0.036(2) 0.058(3) 0.045(2) -0.021(2) 0.010(2) -0.021(2) C36 0.037(3) 0.059(3) 0.047(3) -0.021(2) 0.008(2) -0.023(2) C32 0.034(3) 0.060(3) 0.044(3) -0.020(2) 0.010(2) -0.022(2) C37 0.033(3) 0.078(4) 0.055(4) -0.028(4) 0.007(3) -0.017(3) C40 0.044(4) 0.073(4) 0.055(4) -0.032(3) 0.004(3) -0.023(3) O11B 0.080(3) 0.090(3) 0.086(3) -0.031(3) 0.016(3) -0.021(3) O11A 0.076(3) 0.090(3) 0.102(3) -0.040(3) 0.018(3) -0.024(3) C11 0.083(2) 0.090(2) 0.092(2) -0.0396(19) 0.0153(19) -0.0286(19) O1A 0.081(3) 0.079(3) 0.087(3) -0.038(3) 0.015(3) -0.035(3) O1B 0.081(3) 0.084(3) 0.096(3) -0.031(3) 0.013(3) -0.042(3) C1 0.083(2) 0.082(2) 0.088(2) -0.0369(19) 0.0131(18) -0.0374(18) _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. ; _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 N24 2.288(7) . ? Ag1 N31 2.312(7) . ? Ag1 O11A 2.321(9) 2_757 ? Ag1 O1B 2.512(8) 2_757 ? Ag2 N21 2.275(6) . ? Ag2 O11B 2.301(9) . ? Ag2 O1A 2.397(8) . ? N21 C22 1.300(10) . ? N21 C26 1.350(11) . ? C22 C23 1.395(11) . ? C22 C27 1.498(11) . ? C23 N24 1.333(10) . ? C23 C28 1.503(12) . ? N24 C25 1.335(11) . ? C25 C26 1.385(12) . ? C25 C29 1.502(12) . ? C26 C30 1.506(12) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? N31 C32 1.327(10) . ? N31 C36 1.337(10) . ? C36 C32 1.393(12) 2_758 ? C36 C40 1.509(11) . ? C32 C36 1.393(12) 2_758 ? C32 C37 1.520(11) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? O11B C11 1.226(14) . ? O11A C11 1.213(14) . ? O11A Ag1 2.321(9) 2_757 ? C11 C12 1.5399(10) . ? C11 C12' 1.5402(10) . ? F13Z C13' 1.3498(10) . ? F14Y C14' 1.3500(10) . ? F13Y C13' 1.3498(11) . ? F12Z C12' 1.3500(11) . ? F12Y C12' 1.3500(10) . ? C14' F14Z 1.3499(10) . ? C14' F14X 1.3502(10) . ? C14' C13' 1.5397(10) . ? C12' C13' 1.5395(10) . ? F12B C12 1.3499(11) . ? F12A C12 1.3500(10) . ? F13B C13 1.3500(10) . ? F13A C13 1.3501(11) . ? F14B C14 1.3498(10) . ? C14 F14A 1.3497(10) . ? C14 F14C 1.3498(11) . ? C14 C13 1.5399(10) . ? C12 C13 1.5398(10) . ? O1A C1 1.192(13) . ? O1B C1 1.243(14) . ? O1B Ag1 2.512(8) 2_757 ? C1 C2' 1.5402(10) . ? C1 C2 1.5399(10) . ? F4Z C4' 1.3500(10) . ? F4X C4' 1.3502(10) . ? F4Y C4' 1.3500(10) . ? F2Z C2' 1.3503(10) . ? F3Y C3' 1.3498(10) . ? C2' F2Y 1.3501(10) . ? C2' C3' 1.5397(10) . ? C3' F3Z 1.3499(10) . ? C3' C4' 1.5396(10) . ? C2 F2B 1.3499(11) . ? C2 F2A 1.3499(10) . ? C2 C3 1.5399(10) . ? C3 F3A 1.3499(10) . ? C3 F3B 1.3500(10) . ? C3 C4 1.5398(10) . ? C4 F4A 1.3499(10) . ? C4 F4C 1.3498(11) . ? C4 F4B 1.3499(10) . ? _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 N24 Ag1 N31 122.1(2) . . ? N24 Ag1 O11A 113.3(3) . 2_757 ? N31 Ag1 O11A 115.9(3) . 2_757 ? N24 Ag1 O1B 105.0(3) . 2_757 ? N31 Ag1 O1B 95.6(3) . 2_757 ? O11A Ag1 O1B 99.1(3) 2_757 2_757 ? N21 Ag2 O11B 131.6(3) . . ? N21 Ag2 O1A 128.7(3) . . ? O11B Ag2 O1A 98.2(3) . . ? C22 N21 C26 119.8(7) . . ? C22 N21 Ag2 120.9(5) . . ? C26 N21 Ag2 119.2(5) . . ? N21 C22 C23 120.7(7) . . ? N21 C22 C27 118.2(7) . . ? C23 C22 C27 121.1(7) . . ? N24 C23 C22 120.2(8) . . ? N24 C23 C28 117.7(8) . . ? C22 C23 C28 122.0(8) . . ? C23 N24 C25 119.1(7) . . ? C23 N24 Ag1 119.5(5) . . ? C25 N24 Ag1 121.3(5) . . ? N24 C25 C26 120.3(7) . . ? N24 C25 C29 117.2(7) . . ? C26 C25 C29 122.5(8) . . ? N21 C26 C25 119.8(7) . . ? N21 C26 C30 118.6(8) . . ? C25 C26 C30 121.6(8) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 N31 C36 118.9(7) . . ? C32 N31 Ag1 117.4(5) . . ? C36 N31 Ag1 120.4(5) . . ? N31 C36 C32 120.1(7) . 2_758 ? N31 C36 C40 117.3(8) . . ? C32 C36 C40 122.6(7) 2_758 . ? N31 C32 C36 120.9(7) . 2_758 ? N31 C32 C37 117.4(7) . . ? C36 C32 C37 121.6(7) 2_758 . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C11 O11B Ag2 110.1(6) . . ? C11 O11A Ag1 149.2(8) . 2_757 ? O11A C11 O11B 126.8(8) . . ? O11A C11 C12 114.9(11) . . ? O11B C11 C12 118.3(11) . . ? O11A C11 C12' 117.9(11) . . ? O11B C11 C12' 115.3(11) . . ? F14Y C14' F14Z 106.27(11) . . ? F14Y C14' F14X 106.24(11) . . ? F14Z C14' F14X 116.1(3) . . ? F14Y C14' C13' 109.35(11) . . ? F14Z C14' C13' 109.35(11) . . ? F14X C14' C13' 109.31(11) . . ? F12Y C12' F12Z 106.28(11) . . ? F12Y C12' C13' 96.2(10) . . ? F12Z C12' C13' 120.7(10) . . ? F12Y C12' C11 113.9(12) . . ? F12Z C12' C11 109.0(10) . . ? C13' C12' C11 110.2(7) . . ? F13Z C13' F13Y 106.29(11) . . ? F13Z C13' C12' 118.3(10) . . ? F13Y C13' C12' 105.1(10) . . ? F13Z C13' C14' 109.1(9) . . ? F13Y C13' C14' 100.8(9) . . ? C12' C13' C14' 115.26(11) . . ? F14A C14 F14C 116.0(3) . . ? F14A C14 F14B 106.29(11) . . ? F14C C14 F14B 106.29(11) . . ? F14A C14 C13 109.34(11) . . ? F14C C14 C13 109.33(11) . . ? F14B C14 C13 109.35(11) . . ? F12B C12 F12A 106.28(11) . . ? F12B C12 C13 96.6(11) . . ? F12A C12 C13 124.0(13) . . ? F12B C12 C11 112.7(12) . . ? F12A C12 C11 106.5(12) . . ? C13 C12 C11 110.4(8) . . ? F13B C13 F13A 106.25(11) . . ? F13B C13 C14 117.9(11) . . ? F13A C13 C14 99.9(10) . . ? F13B C13 C12 115.5(12) . . ? F13A C13 C12 97.9(13) . . ? C14 C13 C12 115.19(11) . . ? C1 O1A Ag2 101.7(6) . . ? C1 O1B Ag1 149.5(8) . 2_757 ? O1A C1 O1B 126.6(8) . . ? O1A C1 C2' 112.3(10) . . ? O1B C1 C2' 121.0(10) . . ? O1A C1 C2 124.8(11) . . ? O1B C1 C2 108.6(11) . . ? F2Y C2' F2Z 106.21(11) . . ? F2Y C2' C3' 105.0(8) . . ? F2Z C2' C3' 102.0(8) . . ? F2Y C2' C1 112.7(9) . . ? F2Z C2' C1 111.8(9) . . ? C3' C2' C1 118.0(7) . . ? F3Y C3' F3Z 106.29(11) . . ? F3Y C3' C2' 111.4(9) . . ? F3Z C3' C2' 112.0(9) . . ? F3Y C3' C4' 109.3(9) . . ? F3Z C3' C4' 101.9(10) . . ? C2' C3' C4' 115.23(11) . . ? F4Y C4' F4Z 106.26(11) . . ? F4Y C4' F4X 106.23(11) . . ? F4Z C4' F4X 117.4(11) . . ? F4Y C4' C3' 112.8(10) . . ? F4Z C4' C3' 106.7(8) . . ? F4X C4' C3' 107.7(8) . . ? F2B C2 F2A 106.28(11) . . ? F2B C2 C3 100.4(12) . . ? F2A C2 C3 114.9(13) . . ? F2B C2 C1 112.6(14) . . ? F2A C2 C1 110.3(13) . . ? C3 C2 C1 111.9(11) . . ? F3A C3 F3B 106.27(11) . . ? F3A C3 C4 102.4(16) . . ? F3B C3 C4 102.9(16) . . ? F3A C3 C2 114.1(16) . . ? F3B C3 C2 114.6(15) . . ? C4 C3 C2 115.17(11) . . ? F4A C4 F4C 88(2) . . ? F4A C4 F4B 106.28(11) . . ? F4C C4 F4B 106.28(11) . . ? F4A C4 C3 113.7(17) . . ? F4C C4 C3 124.8(14) . . ? F4B C4 C3 113.8(17) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.312 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.159 data_ilb1340_0m _database_code_depnum_ccdc_archive 'CCDC 903747' #TrackingRef 'SCSC2_step2_1-MeOH_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 Ag4 F28 N6 O10' _chemical_formula_weight 1756.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8383(6) _cell_length_b 12.3906(8) _cell_length_c 15.1371(9) _cell_angle_alpha 109.759(4) _cell_angle_beta 97.132(4) _cell_angle_gamma 104.227(4) _cell_volume 1472.70(16) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 2866 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 22.82 _exptl_crystal_description 'block from a needle' _exptl_crystal_colour colourlees _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 858 _exptl_absorpt_coefficient_mu 1.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6860 _exptl_absorpt_correction_T_max 0.6947 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14217 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0841 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.58 _reflns_number_total 6473 _reflns_number_gt 3127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+1.4040P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6473 _refine_ls_number_parameters 395 _refine_ls_number_restraints 80 _refine_ls_R_factor_all 0.1538 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2708 _refine_ls_wR_factor_gt 0.2129 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O11B O 0.5640(12) 0.1656(8) 0.7630(6) 0.096(3) Uani 1 1 d . . . Ag1 Ag 0.64346(9) 0.77537(7) 1.31645(5) 0.0596(3) Uani 1 1 d . . . Ag2 Ag 0.80937(12) 0.40151(8) 0.87204(6) 0.0724(3) Uani 1 1 d . . . O1A O 1.0353(9) 0.5028(7) 0.8013(6) 0.071(2) Uani 1 1 d . A . O1B O 0.7844(9) 0.4479(7) 0.7269(5) 0.0685(19) Uani 1 1 d . A . C1 C 0.9309(12) 0.4959(8) 0.7379(6) 0.058(3) Uani 1 1 d D . . C2 C 0.9859(14) 0.5489(8) 0.6645(6) 0.064(3) Uiso 0.482(10) 1 d PDU A 1 C3 C 1.0317(15) 0.6871(8) 0.7136(5) 0.087(5) Uiso 0.482(10) 1 d PDU A 1 C4 C 1.0310(19) 0.7539(8) 0.6444(9) 0.111(5) Uiso 0.482(10) 1 d PDU A 1 F4C F 0.950(3) 0.6952(15) 0.5515(11) 0.141(8) Uiso 0.482(10) 1 d PD A 1 F2A F 1.1372(13) 0.5490(15) 0.6589(11) 0.083(4) Uiso 0.482(10) 1 d PDU A 1 F3A F 1.1745(14) 0.7340(16) 0.7776(11) 0.113(5) Uiso 0.482(10) 1 d PDU A 1 F4A F 1.140(2) 0.7340(15) 0.5909(14) 0.118(5) Uiso 0.482(10) 1 d PDU A 1 F2B F 0.8931(14) 0.4802(13) 0.5754(8) 0.079(3) Uiso 0.482(10) 1 d PDU A 1 F3B F 0.9253(16) 0.7259(14) 0.7627(10) 0.089(4) Uiso 0.482(10) 1 d PDU A 1 F4B F 1.040(3) 0.8708(9) 0.6675(14) 0.143(6) Uiso 0.482(10) 1 d PDU A 1 F3Z F 1.0776(17) 0.7479(16) 0.7965(10) 0.125(5) Uiso 0.518(10) 1 d PDU A 2 F2Z F 1.0983(13) 0.5163(15) 0.6309(10) 0.082(3) Uiso 0.518(10) 1 d PDU A 2 F4Z F 1.1990(17) 0.7364(14) 0.6237(14) 0.124(5) Uiso 0.518(10) 1 d PDU A 2 F3Y F 0.8390(14) 0.6908(14) 0.7081(10) 0.096(4) Uiso 0.518(10) 1 d PDU A 2 F4Y F 1.111(2) 0.8763(11) 0.7091(12) 0.131(6) Uiso 0.518(10) 1 d PDU A 2 F2Y F 0.8558(12) 0.5168(13) 0.5894(9) 0.078(3) Uiso 0.518(10) 1 d PDU A 2 F4X F 0.9214(18) 0.7405(16) 0.5915(15) 0.144(7) Uiso 0.518(10) 1 d PD A 2 C2' C 0.9791(14) 0.5539(9) 0.6660(6) 0.064(3) Uiso 0.518(10) 1 d PDU A 2 C3' C 0.9901(16) 0.6882(9) 0.7050(8) 0.089(5) Uiso 0.518(10) 1 d PDU A 2 C4' C 1.0648(14) 0.7599(8) 0.6472(12) 0.111(5) Uiso 0.518(10) 1 d PDU A 2 N21 N 0.6765(9) 0.6553(6) 1.1704(5) 0.0462(17) Uani 1 1 d . . . N24 N 0.7503(9) 0.5172(6) 1.0067(5) 0.0492(18) Uani 1 1 d . . . C23 C 0.7938(11) 0.6388(8) 1.0350(6) 0.046(2) Uani 1 1 d . . . C22 C 0.7540(11) 0.7070(8) 1.1182(6) 0.047(2) Uani 1 1 d . . . C25 C 0.6719(11) 0.4649(7) 1.0595(6) 0.045(2) Uani 1 1 d . . . C26 C 0.6354(10) 0.5337(8) 1.1422(6) 0.045(2) Uani 1 1 d . . . C28 C 0.8827(14) 0.6934(9) 0.9764(7) 0.063(3) Uani 1 1 d . . . H28A H 0.8897 0.6302 0.9195 0.095 Uiso 1 1 calc R . . H28B H 0.9898 0.7428 1.0141 0.095 Uiso 1 1 calc R . . H28C H 0.8271 0.7431 0.9571 0.095 Uiso 1 1 calc R . . C30 C 0.5551(13) 0.4781(9) 1.2057(7) 0.059(2) Uani 1 1 d . . . H30A H 0.6317 0.4554 1.2417 0.089 Uiso 1 1 calc R . . H30B H 0.4658 0.4071 1.1660 0.089 Uiso 1 1 calc R . . H30C H 0.5161 0.5361 1.2502 0.089 Uiso 1 1 calc R . . C27 C 0.7987(13) 0.8431(8) 1.1532(8) 0.061(3) Uani 1 1 d . . . H27A H 0.7183 0.8701 1.1850 0.091 Uiso 1 1 calc R . . H27B H 0.8042 0.8672 1.0987 0.091 Uiso 1 1 calc R . . H27C H 0.9022 0.8791 1.1983 0.091 Uiso 1 1 calc R . . C29 C 0.6313(14) 0.3306(8) 1.0278(8) 0.061(3) Uani 1 1 d . . . H29A H 0.6513 0.2970 0.9641 0.091 Uiso 1 1 calc R . . H29B H 0.5191 0.2965 1.0258 0.091 Uiso 1 1 calc R . . H29C H 0.6972 0.3115 1.0729 0.091 Uiso 1 1 calc R . . O1S O 0.4709(9) 0.7091(8) 1.4087(6) 0.077(2) Uani 1 1 d . . . H1S H 0.3624 0.7044 1.3940 0.116 Uiso 1 1 calc R . . C1S C 0.525(2) 0.6769(15) 1.4838(11) 0.111(5) Uani 1 1 d . . . H1S1 H 0.5382 0.5978 1.4575 0.167 Uiso 1 1 calc R . . H1S2 H 0.4464 0.6751 1.5234 0.167 Uiso 1 1 calc R . . H1S3 H 0.6262 0.7354 1.5228 0.167 Uiso 1 1 calc R . . N31 N 0.8657(9) 0.9124(6) 1.4348(5) 0.0464(17) Uani 1 1 d . . . C32 C 1.0091(10) 0.8945(8) 1.4400(6) 0.046(2) Uani 1 1 d . . . C36 C 0.8596(10) 1.0211(7) 1.4962(6) 0.0425(19) Uani 1 1 d . . . C37 C 1.0146(12) 0.7749(8) 1.3735(7) 0.059(3) Uani 1 1 d . . . H37A H 0.9104 0.7152 1.3570 0.088 Uiso 1 1 calc R . . H37B H 1.0943 0.7503 1.4052 0.088 Uiso 1 1 calc R . . H37C H 1.0427 0.7818 1.3153 0.088 Uiso 1 1 calc R . . C40 C 0.6960(12) 1.0355(10) 1.4896(8) 0.070(3) Uani 1 1 d . . . H40A H 0.6889 1.0884 1.5519 0.105 Uiso 1 1 calc R . . H40B H 0.6164 0.9573 1.4704 0.105 Uiso 1 1 calc R . . H40C H 0.6764 1.0701 1.4422 0.105 Uiso 1 1 calc R . . O11A O 0.8213(10) 0.2054(7) 0.8256(6) 0.072(2) Uani 1 1 d . B . C11 C 0.6836(14) 0.1376(6) 0.7811(7) 0.059(3) Uani 1 1 d D . . F12A F 0.8133(10) -0.0150(10) 0.7307(8) 0.087(3) Uiso 0.643(11) 1 d PDU B 1 F13A F 0.5816(16) -0.1849(8) 0.7758(10) 0.121(5) Uiso 0.643(11) 1 d PD B 1 F12B F 0.5610(12) -0.0633(12) 0.6652(7) 0.109(4) Uiso 0.643(11) 1 d PDU B 1 F13B F 0.4731(14) -0.0465(12) 0.8367(11) 0.131(5) Uiso 0.643(11) 1 d PD B 1 F14A F 0.6457(13) -0.0915(8) 0.9573(6) 0.114(5) Uiso 0.643(11) 1 d PD B 1 F14B F 0.7298(13) 0.0903(6) 0.9631(6) 0.103(4) Uiso 0.643(11) 1 d PD B 1 F14C F 0.8656(9) -0.0274(11) 0.9009(8) 0.152(7) Uiso 0.643(11) 1 d PD B 1 C13 C 0.6080(9) -0.0645(7) 0.8100(5) 0.088(5) Uiso 0.643(11) 1 d PDU B 1 C12 C 0.6736(10) 0.0036(6) 0.7477(5) 0.075(3) Uiso 0.643(11) 1 d PDU B 1 C14 C 0.7164(8) -0.0252(6) 0.9104(5) 0.141(9) Uiso 0.643(11) 1 d PDU B 1 F14Z F 0.607(2) 0.0730(14) 0.9397(12) 0.103(7) Uiso 0.357(11) 1 d PD B 2 F12Z F 0.7597(18) -0.0277(18) 0.6871(14) 0.089(5) Uiso 0.357(11) 1 d PDU B 2 F13Z F 0.669(2) -0.1771(11) 0.7758(15) 0.092(7) Uiso 0.357(11) 1 d PD B 2 F12Y F 0.5102(16) -0.064(2) 0.6933(16) 0.104(5) Uiso 0.357(11) 1 d PDU B 2 F14Y F 0.4369(18) -0.101(2) 0.8501(18) 0.26(3) Uiso 0.357(11) 1 d PD B 2 C13' C 0.6947(16) -0.0572(12) 0.8179(10) 0.087(6) Uiso 0.357(11) 1 d PDU B 2 C12' C 0.6604(19) 0.0014(6) 0.7458(9) 0.075(4) Uiso 0.357(11) 1 d PDU B 2 F13Y F 0.850(2) -0.0084(18) 0.865(2) 0.143(11) Uiso 0.357(11) 1 d PD B 2 F14X F 0.631(4) -0.102(3) 0.951(2) 0.62(10) Uiso 0.357(11) 1 d PD B 2 C14' C 0.5931(19) -0.0445(12) 0.8943(11) 0.142(9) Uiso 0.357(11) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O11B 0.115(7) 0.093(6) 0.087(6) 0.032(5) 0.003(5) 0.056(6) Ag1 0.0572(5) 0.0545(5) 0.0579(5) 0.0130(4) 0.0117(3) 0.0141(4) Ag2 0.1071(7) 0.0574(5) 0.0624(5) 0.0245(4) 0.0341(5) 0.0326(5) O1A 0.062(4) 0.080(5) 0.073(5) 0.034(4) 0.012(4) 0.022(4) O1B 0.062(5) 0.072(5) 0.062(4) 0.026(4) 0.007(3) 0.007(4) C1 0.053(6) 0.054(6) 0.059(6) 0.010(5) 0.011(5) 0.018(5) N21 0.051(4) 0.046(4) 0.047(4) 0.019(3) 0.016(3) 0.019(4) N24 0.060(5) 0.039(4) 0.050(4) 0.021(3) 0.009(3) 0.013(4) C23 0.052(5) 0.045(5) 0.044(5) 0.017(4) 0.009(4) 0.019(4) C22 0.047(5) 0.040(5) 0.051(5) 0.016(4) 0.003(4) 0.014(4) C25 0.051(5) 0.036(4) 0.048(5) 0.020(4) 0.007(4) 0.010(4) C26 0.044(5) 0.040(5) 0.050(5) 0.019(4) 0.007(4) 0.013(4) C28 0.086(8) 0.048(6) 0.060(6) 0.026(5) 0.022(5) 0.019(6) C30 0.070(6) 0.047(5) 0.062(6) 0.022(5) 0.027(5) 0.015(5) C27 0.060(6) 0.043(5) 0.070(6) 0.022(5) 0.008(5) 0.004(5) C29 0.081(7) 0.040(5) 0.068(6) 0.023(5) 0.028(5) 0.022(5) O1S 0.062(4) 0.092(6) 0.076(5) 0.038(4) 0.018(4) 0.014(4) C1S 0.123(13) 0.104(11) 0.092(10) 0.048(9) 0.004(9) 0.006(10) N31 0.049(4) 0.038(4) 0.052(4) 0.019(3) 0.013(3) 0.012(3) C32 0.039(5) 0.048(5) 0.049(5) 0.018(4) 0.010(4) 0.011(4) C36 0.043(5) 0.042(5) 0.040(4) 0.011(4) 0.008(4) 0.018(4) C37 0.060(6) 0.041(5) 0.067(6) 0.006(4) 0.010(5) 0.022(5) C40 0.054(6) 0.070(7) 0.074(7) 0.008(6) 0.015(5) 0.026(6) O11A 0.076(5) 0.059(5) 0.079(5) 0.023(4) 0.016(4) 0.025(4) C11 0.068(7) 0.061(6) 0.059(6) 0.032(5) 0.013(5) 0.026(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 O11B C11 1.219(12) . ? O11B Ag1 2.459(9) 2_667 ? Ag1 N21 2.310(7) . ? Ag1 N31 2.320(7) . ? Ag1 O1S 2.374(8) . ? Ag1 O11B 2.459(9) 2_667 ? Ag2 N24 2.266(7) . ? Ag2 O11A 2.323(7) . ? Ag2 O1B 2.449(7) . ? O1A C1 1.211(11) . ? O1B C1 1.249(11) . ? C1 C2 1.5396(10) . ? C1 C2' 1.5405(10) . ? C2 F2B 1.3498(10) . ? C2 F2A 1.3499(10) . ? C2 C3 1.5400(10) . ? C3 F3A 1.3499(11) . ? C3 F3B 1.3501(10) . ? C3 C4 1.5398(10) . ? C4 F4B 1.3495(11) . ? C4 F4A 1.3498(10) . ? C4 F4C 1.3499(10) . ? F3Z C3' 1.3498(10) . ? F2Z C2' 1.3503(10) . ? F4Z C4' 1.3501(10) . ? F3Y C3' 1.3497(10) . ? F4Y C4' 1.3506(10) . ? F2Y C2' 1.3502(10) . ? F4X C4' 1.3504(10) . ? C2' C3' 1.5396(10) . ? C3' C4' 1.5395(10) . ? N21 C22 1.329(12) . ? N21 C26 1.357(11) . ? N24 C25 1.343(11) . ? N24 C23 1.357(11) . ? C23 C22 1.400(12) . ? C23 C28 1.476(14) . ? C22 C27 1.515(12) . ? C25 C26 1.384(12) . ? C25 C29 1.500(12) . ? C26 C30 1.509(13) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? O1S C1S 1.394(16) . ? O1S H1S 0.9400 . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C1S H1S3 0.9700 . ? N31 C32 1.337(11) . ? N31 C36 1.372(10) . ? C32 C36 1.348(12) 2_778 ? C32 C37 1.500(12) . ? C36 C32 1.348(12) 2_778 ? C36 C40 1.496(12) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? O11A C11 1.246(12) . ? C11 C12' 1.5399(10) . ? C11 C12 1.5402(10) . ? F12A C12 1.3500(10) . ? F13A C13 1.3501(10) . ? F12B C12 1.3502(10) . ? F13B C13 1.3499(10) . ? F14A C14 1.3501(10) . ? F14B C14 1.3498(10) . ? F14C C14 1.3499(10) . ? C13 C12 1.5397(10) . ? C13 C14 1.5399(10) . ? F14Z C14' 1.3501(10) . ? F12Z C12' 1.3498(10) . ? F13Z C13' 1.3499(10) . ? F12Y C12' 1.3499(11) . ? F14Y C14' 1.3501(11) . ? C13' F13Y 1.3499(11) . ? C13' C12' 1.5399(10) . ? C13' C14' 1.5403(10) . ? F14X C14' 1.3501(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 O11B Ag1 162.4(9) . 2_667 ? N21 Ag1 N31 119.9(3) . . ? N21 Ag1 O1S 125.6(3) . . ? N31 Ag1 O1S 102.2(3) . . ? N21 Ag1 O11B 92.1(3) . 2_667 ? N31 Ag1 O11B 123.5(3) . 2_667 ? O1S Ag1 O11B 91.6(3) . 2_667 ? N24 Ag2 O11A 129.9(3) . . ? N24 Ag2 O1B 120.4(3) . . ? O11A Ag2 O1B 107.2(3) . . ? C1 O1B Ag2 95.8(5) . . ? O1A C1 O1B 125.1(7) . . ? O1A C1 C2 116.6(9) . . ? O1B C1 C2 118.3(9) . . ? O1A C1 C2' 118.5(9) . . ? O1B C1 C2' 116.3(9) . . ? F2B C2 F2A 106.29(11) . . ? F2B C2 C1 110.4(10) . . ? F2A C2 C1 110.8(11) . . ? F2B C2 C3 126.1(9) . . ? F2A C2 C3 94.2(10) . . ? C1 C2 C3 107.5(7) . . ? F3A C3 F3B 106.27(11) . . ? F3A C3 C4 109.6(13) . . ? F3B C3 C4 99.4(11) . . ? F3A C3 C2 111.6(11) . . ? F3B C3 C2 113.9(11) . . ? C4 C3 C2 115.16(11) . . ? F4B C4 F4A 106.31(11) . . ? F4B C4 F4C 106.31(11) . . ? F4A C4 F4C 72.9(15) . . ? F4B C4 C3 126.8(10) . . ? F4A C4 C3 109.9(14) . . ? F4C C4 C3 120.7(11) . . ? F2Y C2' F2Z 106.21(11) . . ? F2Y C2' C3' 97.2(10) . . ? F2Z C2' C3' 121.5(10) . . ? F2Y C2' C1 110.7(10) . . ? F2Z C2' C1 109.1(11) . . ? C3' C2' C1 111.1(8) . . ? F3Y C3' F3Z 106.30(11) . . ? F3Y C3' C4' 111.5(12) . . ? F3Z C3' C4' 105.6(13) . . ? F3Y C3' C2' 105.6(11) . . ? F3Z C3' C2' 112.3(12) . . ? C4' C3' C2' 115.27(11) . . ? F4Z C4' F4X 131.1(16) . . ? F4Z C4' F4Y 106.18(11) . . ? F4X C4' F4Y 106.19(11) . . ? F4Z C4' C3' 112.7(12) . . ? F4X C4' C3' 93.2(13) . . ? F4Y C4' C3' 104.6(13) . . ? C22 N21 C26 119.1(7) . . ? C22 N21 Ag1 119.2(6) . . ? C26 N21 Ag1 121.3(6) . . ? C25 N24 C23 119.5(8) . . ? C25 N24 Ag2 119.7(6) . . ? C23 N24 Ag2 120.8(6) . . ? N24 C23 C22 119.1(9) . . ? N24 C23 C28 118.1(8) . . ? C22 C23 C28 122.9(8) . . ? N21 C22 C23 121.4(8) . . ? N21 C22 C27 117.0(8) . . ? C23 C22 C27 121.5(9) . . ? N24 C25 C26 120.7(8) . . ? N24 C25 C29 117.9(8) . . ? C26 C25 C29 121.4(8) . . ? N21 C26 C25 120.2(8) . . ? N21 C26 C30 117.9(8) . . ? C25 C26 C30 121.9(8) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C1S O1S Ag1 122.5(9) . . ? C1S O1S H1S 118.8 . . ? Ag1 O1S H1S 118.8 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C32 N31 C36 116.9(7) . . ? C32 N31 Ag1 121.5(6) . . ? C36 N31 Ag1 121.3(5) . . ? N31 C32 C36 121.2(8) . 2_778 ? N31 C32 C37 116.6(8) . . ? C36 C32 C37 122.2(8) 2_778 . ? C32 C36 N31 122.0(7) 2_778 . ? C32 C36 C40 123.2(8) 2_778 . ? N31 C36 C40 114.8(8) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C11 O11A Ag2 106.7(5) . . ? O11B C11 O11A 128.1(8) . . ? O11B C11 C12' 115.7(11) . . ? O11A C11 C12' 116.2(10) . . ? O11B C11 C12 119.8(9) . . ? O11A C11 C12 112.1(8) . . ? F13B C13 F13A 106.27(11) . . ? F13B C13 C12 115.1(10) . . ? F13A C13 C12 117.5(9) . . ? F13B C13 C14 99.3(8) . . ? F13A C13 C14 101.1(8) . . ? C12 C13 C14 115.20(11) . . ? F12A C12 F12B 106.94(11) . . ? F12A C12 C13 109.8(8) . . ? F12B C12 C13 98.1(8) . . ? F12A C12 C11 112.4(9) . . ? F12B C12 C11 111.2(9) . . ? C13 C12 C11 117.1(7) . . ? F14B C14 F14C 106.26(11) . . ? F14B C14 F14A 106.27(11) . . ? F14C C14 F14A 116.1(3) . . ? F14B C14 C13 109.34(11) . . ? F14C C14 C13 109.34(11) . . ? F14A C14 C13 109.31(11) . . ? F13Z C13' F13Y 106.29(11) . . ? F13Z C13' C12' 113.6(13) . . ? F13Y C13' C12' 109.4(19) . . ? F13Z C13' C14' 104.2(14) . . ? F13Y C13' C14' 107.7(18) . . ? C12' C13' C14' 115.14(11) . . ? F12Z C12' F12Y 106.29(11) . . ? F12Z C12' C13' 101.9(13) . . ? F12Y C12' C13' 105.3(14) . . ? F12Z C12' C11 110.1(13) . . ? F12Y C12' C11 111.4(16) . . ? C13' C12' C11 120.6(10) . . ? F14X C14' F14Y 106.24(11) . . ? F14X C14' F14Z 116.3(3) . . ? F14Y C14' F14Z 106.25(11) . . ? F14X C14' C13' 109.29(11) . . ? F14Y C14' C13' 109.29(11) . . ? F14Z C14' C13' 109.27(11) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.192 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.163 data_ilb1342 _database_code_depnum_ccdc_archive 'CCDC 903748' #TrackingRef 'SCSC2_step3_1_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 Ag4 F28 N6 O8' _chemical_formula_weight 1692.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5117(4) _cell_length_b 12.8936(7) _cell_length_c 14.8429(11) _cell_angle_alpha 112.463(5) _cell_angle_beta 90.650(4) _cell_angle_gamma 109.191(3) _cell_volume 1404.09(14) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 6252 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 23.18 _exptl_crystal_description 'block from a needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.001 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 1.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6756 _exptl_absorpt_correction_T_max 0.6844 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20357 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.1117 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.62 _reflns_number_total 6386 _reflns_number_gt 2624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1278P)^2^+9.4499P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6386 _refine_ls_number_parameters 366 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.1948 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.2905 _refine_ls_wR_factor_gt 0.2002 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.57248(13) 0.42914(10) 0.20785(8) 0.0649(4) Uani 1 1 d . . . Ag2 Ag 0.89234(14) 0.48445(9) 0.37662(8) 0.0673(4) Uani 1 1 d . . . N21 N 0.4126(11) 0.4562(8) 0.3320(6) 0.043(2) Uani 1 1 d . . . N24 N 0.7645(11) 0.5135(8) 0.5128(6) 0.042(2) Uani 1 1 d . . . C23 C 0.7699(14) 0.6204(9) 0.5716(8) 0.046(3) Uani 1 1 d . . . C22 C 0.3169(14) 0.3625(10) 0.3485(8) 0.046(3) Uani 1 1 d . . . C26 C 0.6719(14) 0.4186(9) 0.5294(8) 0.046(3) Uani 1 1 d . . . C25 C 0.4183(14) 0.5679(10) 0.3922(9) 0.050(3) Uani 1 1 d . . . C30 C 0.6634(18) 0.2943(11) 0.4610(10) 0.067(4) Uani 1 1 d . . . H30A H 0.7040 0.2964 0.4007 0.101 Uiso 1 1 calc R . . H30B H 0.5478 0.2387 0.4454 0.101 Uiso 1 1 calc R . . H30C H 0.7331 0.2681 0.4930 0.101 Uiso 1 1 calc R . . C28 C 0.8827(18) 0.7258(11) 0.5545(10) 0.066(4) Uani 1 1 d . . . H28A H 0.9486 0.6989 0.5037 0.099 Uiso 1 1 calc R . . H28B H 0.9576 0.7845 0.6152 0.099 Uiso 1 1 calc R . . H28C H 0.8148 0.7623 0.5334 0.099 Uiso 1 1 calc R . . C27 C 0.3086(17) 0.2395(11) 0.2781(9) 0.063(3) Uani 1 1 d . . . H27A H 0.3543 0.2443 0.2196 0.095 Uiso 1 1 calc R . . H27B H 0.1924 0.1845 0.2593 0.095 Uiso 1 1 calc R . . H27C H 0.3740 0.2103 0.3100 0.095 Uiso 1 1 calc R . . C29 C 0.5136(16) 0.6685(10) 0.3640(10) 0.062(3) Uani 1 1 d . . . H29A H 0.5725 0.6391 0.3099 0.093 Uiso 1 1 calc R . . H29B H 0.5944 0.7329 0.4202 0.093 Uiso 1 1 calc R . . H29C H 0.4356 0.6987 0.3435 0.093 Uiso 1 1 calc R . . N31 N 0.5087(11) 0.4491(8) 0.0656(7) 0.047(2) Uani 1 1 d . . . C33 C 0.6258(13) 0.5241(10) -0.0514(8) 0.046(3) Uani 1 1 d . . . C32 C 0.6323(13) 0.4701(10) 0.0126(8) 0.047(3) Uani 1 1 d . . . C38 C 0.7665(15) 0.5544(13) -0.1077(9) 0.061(3) Uani 1 1 d . . . H38A H 0.7758 0.4808 -0.1549 0.092 Uiso 1 1 calc R . . H38B H 0.8714 0.6027 -0.0621 0.092 Uiso 1 1 calc R . . H38C H 0.7433 0.5993 -0.1424 0.092 Uiso 1 1 calc R . . C37 C 0.7774(15) 0.4334(13) 0.0269(10) 0.063(3) Uani 1 1 d . . . H37A H 0.8814 0.5026 0.0468 0.094 Uiso 1 1 calc R . . H37B H 0.7826 0.3713 -0.0345 0.094 Uiso 1 1 calc R . . H37C H 0.7619 0.4025 0.0777 0.094 Uiso 1 1 calc R . . O11B O 0.8383(12) 0.6108(9) 0.2717(9) 0.090(3) Uani 1 1 d . A . O11A O 1.0870(12) 0.6309(9) 0.3302(8) 0.077(3) Uani 1 1 d . A . C11 C 0.9887(18) 0.6541(10) 0.2883(9) 0.062(3) Uiso 1 1 d D . . C12 C 1.0876(12) 0.7457(8) 0.2476(5) 0.098(11) Uiso 0.668(17) 1 d PD A 1 F12A F 1.0079(16) 0.7316(13) 0.1622(8) 0.098(5) Uiso 0.668(17) 1 d PD A 1 C14 C 1.2301(11) 0.9382(7) 0.4085(6) 0.083(7) Uiso 0.668(17) 1 d PD A 1 C13 C 1.1111(14) 0.8781(8) 0.3093(7) 0.26(3) Uiso 0.668(17) 1 d PD A 1 F12B F 1.2453(13) 0.7493(12) 0.2331(9) 0.082(4) Uiso 0.668(17) 1 d PD A 1 F13B F 1.206(2) 0.9508(16) 0.2695(14) 0.144(7) Uiso 0.668(17) 1 d PD A 1 F14B F 1.3783(11) 0.9227(13) 0.3928(9) 0.139(7) Uiso 0.668(17) 1 d PD A 1 F14A F 1.1647(17) 0.8822(12) 0.4673(7) 0.116(6) Uiso 0.668(17) 1 d PD A 1 F13A F 0.971(2) 0.906(2) 0.325(2) 0.179(10) Uiso 0.668(17) 1 d PD A 1 F14C F 1.265(2) 1.0581(7) 0.4462(10) 0.162(9) Uiso 0.668(17) 1 d PD A 1 F13Z F 0.960(2) 0.886(2) 0.358(2) 0.094(10) Uiso 0.332(17) 1 d PD A 2 F14Z F 1.045(3) 0.860(2) 0.4640(12) 0.29(4) Uiso 0.332(17) 1 d PD A 2 F12Z F 0.933(2) 0.746(3) 0.189(2) 0.117(11) Uiso 0.332(17) 1 d PD A 2 F12Y F 1.182(2) 0.739(2) 0.1959(18) 0.079(8) Uiso 0.332(17) 1 d PD A 2 F14Y F 1.300(2) 0.8927(18) 0.4333(14) 0.154(16) Uiso 0.332(17) 1 d PD A 2 F14X F 1.219(3) 1.0445(12) 0.4749(13) 0.077(8) Uiso 0.332(17) 1 d PD A 2 F13Y F 1.120(4) 0.957(2) 0.2673(19) 0.097(10) Uiso 0.332(17) 1 d PD A 2 C12' C 1.059(2) 0.7532(9) 0.2500(9) 0.046(11) Uiso 0.332(17) 1 d PD A 2 C14' C 1.1648(16) 0.9236(12) 0.4267(9) 0.7(3) Uiso 0.332(17) 1 d PD A 2 C13' C 1.102(2) 0.8871(10) 0.3174(10) 0.032(8) Uiso 0.332(17) 1 d PD A 2 O1A O 0.9303(14) 0.3159(9) 0.2641(7) 0.085(3) Uani 1 1 d . B . O1B O 0.6846(13) 0.2820(10) 0.1887(10) 0.101(4) Uani 1 1 d . B . C1 C 0.8066(19) 0.2570(9) 0.1984(9) 0.069(4) Uiso 1 1 d D . . C2 C 0.7999(16) 0.1333(8) 0.1233(9) 0.056(13) Uiso 0.50(2) 1 d PD B 1 F2A F 0.9492(18) 0.1183(17) 0.1267(13) 0.081(6) Uiso 0.50(2) 1 d PD B 1 C3 C 0.6973(18) 0.0318(12) 0.1532(9) 0.12(3) Uiso 0.50(2) 1 d PD B 1 F3A F 0.719(3) 0.060(2) 0.2510(10) 0.121(8) Uiso 0.50(2) 1 d PD B 1 F2B F 0.766(3) 0.131(2) 0.0332(13) 0.116(8) Uiso 0.50(2) 1 d PD B 1 F3B F 0.540(2) 0.0263(18) 0.1295(14) 0.105(7) Uiso 0.50(2) 1 d PD B 1 C4 C 0.700(2) -0.0936(9) 0.0892(12) 0.089(12) Uiso 0.50(2) 1 d PD B 1 F4A F 0.838(3) -0.110(4) 0.118(2) 0.208(17) Uiso 0.50(2) 1 d PD B 1 F4B F 0.706(3) -0.104(3) -0.0047(14) 0.152(11) Uiso 0.50(2) 1 d PD B 1 F4C F 0.547(3) -0.169(3) 0.089(3) 0.247(19) Uiso 0.50(2) 1 d PD B 1 F3Z F 0.819(2) 0.0564(18) 0.2403(14) 0.099(7) Uiso 0.50(2) 1 d PD B 2 F2Z F 0.9634(16) 0.1483(18) 0.0990(13) 0.083(6) Uiso 0.50(2) 1 d PD B 2 F4Z F 0.8533(17) -0.094(3) 0.075(2) 0.165(12) Uiso 0.50(2) 1 d PD B 2 F3Y F 0.562(2) 0.025(3) 0.1881(18) 0.153(11) Uiso 0.50(2) 1 d PD B 2 F4Y F 0.600(3) -0.142(2) 0.0054(17) 0.162(12) Uiso 0.50(2) 1 d PD B 2 F2Y F 0.7015(19) 0.090(2) 0.0390(16) 0.111(8) Uiso 0.50(2) 1 d PD B 2 F4X F 0.640(3) -0.1648(18) 0.1396(16) 0.138(10) Uiso 0.50(2) 1 d PD B 2 C2' C 0.808(2) 0.1354(8) 0.1241(10) 0.13(3) Uiso 0.50(2) 1 d PD B 2 C3' C 0.716(2) 0.0387(12) 0.1614(9) 0.10(3) Uiso 0.50(2) 1 d PD B 2 C4' C 0.700(2) -0.0905(10) 0.0938(14) 0.37(8) Uiso 0.50(2) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0702(7) 0.0767(8) 0.0690(7) 0.0412(6) 0.0248(5) 0.0384(6) Ag2 0.0792(8) 0.0647(7) 0.0618(7) 0.0266(5) 0.0208(5) 0.0294(6) N21 0.040(5) 0.040(5) 0.047(5) 0.016(4) 0.002(4) 0.014(4) N24 0.046(5) 0.042(5) 0.040(5) 0.020(4) 0.010(4) 0.013(4) C23 0.050(7) 0.034(6) 0.053(7) 0.014(5) 0.001(5) 0.017(5) C22 0.043(6) 0.044(6) 0.049(7) 0.020(5) 0.005(5) 0.014(5) C26 0.048(7) 0.033(6) 0.051(7) 0.013(5) -0.003(5) 0.013(5) C25 0.044(6) 0.039(6) 0.063(7) 0.025(6) 0.001(6) 0.008(5) C30 0.078(9) 0.045(7) 0.064(8) 0.008(6) 0.011(7) 0.023(7) C28 0.091(10) 0.046(7) 0.068(8) 0.032(6) 0.025(7) 0.022(7) C27 0.069(9) 0.044(7) 0.062(8) 0.008(6) 0.006(7) 0.019(6) C29 0.067(8) 0.038(6) 0.081(9) 0.026(6) 0.029(7) 0.014(6) N31 0.039(5) 0.054(6) 0.049(5) 0.018(5) 0.004(4) 0.022(4) C33 0.038(6) 0.046(6) 0.044(6) 0.011(5) 0.005(5) 0.012(5) C32 0.038(6) 0.050(7) 0.050(7) 0.018(6) 0.002(5) 0.016(5) C38 0.050(7) 0.090(10) 0.068(8) 0.049(8) 0.022(6) 0.035(7) C37 0.054(7) 0.082(9) 0.072(9) 0.034(7) 0.018(6) 0.046(7) O11B 0.048(6) 0.078(7) 0.125(9) 0.031(7) 0.003(6) 0.012(5) O11A 0.065(6) 0.081(7) 0.091(7) 0.040(6) 0.010(5) 0.028(5) O1A 0.111(8) 0.072(7) 0.070(6) 0.011(5) 0.009(6) 0.052(6) O1B 0.078(7) 0.095(8) 0.163(11) 0.060(8) 0.019(7) 0.060(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 N21 2.291(9) . ? Ag1 N31 2.303(9) . ? Ag1 O1B 2.318(10) . ? Ag1 O11B 2.505(9) . ? Ag1 Ag2 3.3763(16) . ? Ag2 N24 2.270(8) . ? Ag2 O1A 2.306(9) . ? Ag2 O11A 2.397(10) . ? N21 C22 1.329(13) . ? N21 C25 1.358(14) . ? N24 C23 1.305(13) . ? N24 C26 1.334(13) . ? C23 C22 1.388(15) 2_666 ? C23 C28 1.499(16) . ? C22 C23 1.388(15) 2_666 ? C22 C27 1.508(16) . ? C26 C25 1.388(16) 2_666 ? C26 C30 1.511(15) . ? C25 C26 1.388(16) 2_666 ? C25 C29 1.499(15) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? N31 C33 1.336(13) 2_665 ? N31 C32 1.339(13) . ? C33 N31 1.336(13) 2_665 ? C33 C32 1.386(16) . ? C33 C38 1.500(15) . ? C32 C37 1.499(15) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? O11B C11 1.195(15) . ? O11A C11 1.214(15) . ? C11 C12 1.5400(10) . ? C11 C12' 1.5400(10) . ? C12 F12B 1.3500(10) . ? C12 F12A 1.3500(10) . ? C12 C13 1.5398(10) . ? C14 F14A 1.3498(10) . ? C14 F14B 1.3498(10) . ? C14 F14C 1.3499(10) . ? C14 C13 1.5396(10) . ? C13 F13A 1.3498(10) . ? C13 F13B 1.3500(10) . ? F13Z C13' 1.3500(10) . ? F14Z C14' 1.3499(10) . ? F12Z C12' 1.3501(10) . ? F12Y C12' 1.3500(10) . ? F14Y C14' 1.3499(10) . ? F14X C14' 1.3500(10) . ? F13Y C13' 1.3499(10) . ? C12' C13' 1.5398(10) . ? C14' C13' 1.5397(10) . ? O1A C1 1.234(16) . ? O1B C1 1.206(16) . ? C1 C2' 1.5400(10) . ? C1 C2 1.5401(10) . ? C2 F2B 1.3501(10) . ? C2 F2A 1.3500(10) . ? C2 C3 1.5399(10) . ? C3 F3A 1.3500(10) . ? C3 F3B 1.3500(10) . ? C3 C4 1.5400(10) . ? C4 F4C 1.3498(10) . ? C4 F4A 1.3498(10) . ? C4 F4B 1.3499(10) . ? F3Z C3' 1.3498(10) . ? F2Z C2' 1.3499(10) . ? F4Z C4' 1.3499(10) . ? F3Y C3' 1.3498(10) . ? F4Y C4' 1.3499(10) . ? F2Y C2' 1.3499(10) . ? F4X C4' 1.3500(10) . ? C2' C3' 1.5397(10) . ? C3' C4' 1.5398(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Ag1 N31 122.2(3) . . ? N21 Ag1 O1B 113.2(4) . . ? N31 Ag1 O1B 115.6(4) . . ? N21 Ag1 O11B 105.5(3) . . ? N31 Ag1 O11B 95.4(4) . . ? O1B Ag1 O11B 99.3(4) . . ? N21 Ag1 Ag2 87.7(2) . . ? N31 Ag1 Ag2 143.8(2) . . ? O1B Ag1 Ag2 60.3(3) . . ? O11B Ag1 Ag2 53.9(3) . . ? N24 Ag2 O1A 131.5(4) . . ? N24 Ag2 O11A 129.0(3) . . ? O1A Ag2 O11A 98.0(4) . . ? N24 Ag2 Ag1 100.1(2) . . ? O1A Ag2 Ag1 87.0(3) . . ? O11A Ag2 Ag1 92.9(2) . . ? C22 N21 C25 118.8(9) . . ? C22 N21 Ag1 120.2(7) . . ? C25 N21 Ag1 121.0(7) . . ? C23 N24 C26 119.1(9) . . ? C23 N24 Ag2 121.3(7) . . ? C26 N24 Ag2 119.4(7) . . ? N24 C23 C22 121.4(10) . 2_666 ? N24 C23 C28 117.8(10) . . ? C22 C23 C28 120.6(10) 2_666 . ? N21 C22 C23 120.3(10) . 2_666 ? N21 C22 C27 117.4(10) . . ? C23 C22 C27 122.3(10) 2_666 . ? N24 C26 C25 121.1(10) . 2_666 ? N24 C26 C30 119.4(10) . . ? C25 C26 C30 119.5(10) 2_666 . ? N21 C25 C26 119.2(9) . 2_666 ? N21 C25 C29 116.5(10) . . ? C26 C25 C29 124.1(10) 2_666 . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C33 N31 C32 118.2(10) 2_665 . ? C33 N31 Ag1 121.0(7) 2_665 . ? C32 N31 Ag1 117.7(7) . . ? N31 C33 C32 120.6(9) 2_665 . ? N31 C33 C38 117.2(10) 2_665 . ? C32 C33 C38 122.2(10) . . ? N31 C32 C33 121.1(10) . . ? N31 C32 C37 116.7(10) . . ? C33 C32 C37 122.2(10) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C11 O11B Ag1 150.1(9) . . ? C11 O11A Ag2 99.8(7) . . ? O11B C11 O11A 129.0(10) . . ? O11B C11 C12 121.5(12) . . ? O11A C11 C12 109.3(11) . . ? O11B C11 C12' 112.3(14) . . ? O11A C11 C12' 118.7(13) . . ? F12B C12 F12A 106.97(11) . . ? F12B C12 C13 103.8(9) . . ? F12A C12 C13 98.7(9) . . ? F12B C12 C11 115.7(11) . . ? F12A C12 C11 113.5(9) . . ? C13 C12 C11 116.4(8) . . ? F14A C14 F14B 106.29(11) . . ? F14A C14 F14C 116.0(3) . . ? F14B C14 F14C 106.27(11) . . ? F14A C14 C13 109.37(11) . . ? F14B C14 C13 109.35(11) . . ? F14C C14 C13 109.35(11) . . ? F13A C13 F13B 106.29(11) . . ? F13A C13 C14 108.2(14) . . ? F13B C13 C14 95.5(11) . . ? F13A C13 C12 117.8(13) . . ? F13B C13 C12 111.3(12) . . ? C14 C13 C12 115.21(11) . . ? F12Y C12' F12Z 106.25(11) . . ? F12Y C12' C13' 110.2(16) . . ? F12Z C12' C13' 95.2(16) . . ? F12Y C12' C11 112.9(16) . . ? F12Z C12' C11 108.1(19) . . ? C13' C12' C11 121.7(9) . . ? F14Y C14' F14Z 106.28(11) . . ? F14Y C14' F14X 106.27(11) . . ? F14Z C14' F14X 116.0(3) . . ? F14Y C14' C13' 109.34(11) . . ? F14Z C14' C13' 109.34(11) . . ? F14X C14' C13' 109.33(11) . . ? F13Y C13' F13Z 106.27(11) . . ? F13Y C13' C14' 129.0(16) . . ? F13Z C13' C14' 78.1(14) . . ? F13Y C13' C12' 113.4(14) . . ? F13Z C13' C12' 102.0(18) . . ? C14' C13' C12' 115.21(11) . . ? C1 O1A Ag2 109.6(7) . . ? C1 O1B Ag1 148.4(10) . . ? O1B C1 O1A 127.6(10) . . ? O1B C1 C2' 117.7(14) . . ? O1A C1 C2' 114.7(12) . . ? O1B C1 C2 115.4(13) . . ? O1A C1 C2 116.9(12) . . ? F2B C2 F2A 106.25(11) . . ? F2B C2 C3 122.1(16) . . ? F2A C2 C3 98.1(12) . . ? F2B C2 C1 106.1(15) . . ? F2A C2 C1 112.9(13) . . ? C3 C2 C1 111.3(10) . . ? F3A C3 F3B 106.26(11) . . ? F3A C3 C2 114.8(14) . . ? F3B C3 C2 99.7(14) . . ? F3A C3 C4 113.5(14) . . ? F3B C3 C4 105.4(15) . . ? C2 C3 C4 115.18(11) . . ? F4C C4 F4A 119(2) . . ? F4C C4 F4B 106.28(11) . . ? F4A C4 F4B 106.28(11) . . ? F4C C4 C3 104(2) . . ? F4A C4 C3 113(2) . . ? F4B C4 C3 108.7(14) . . ? F2Y C2' F2Z 106.28(11) . . ? F2Y C2' C3' 97.2(15) . . ? F2Z C2' C3' 121.5(16) . . ? F2Y C2' C1 113.3(17) . . ? F2Z C2' C1 110.0(13) . . ? C3' C2' C1 108.0(10) . . ? F3Y C3' F3Z 106.29(11) . . ? F3Y C3' C2' 122.7(17) . . ? F3Z C3' C2' 107.2(16) . . ? F3Y C3' C4' 103.2(17) . . ? F3Z C3' C4' 99.6(15) . . ? C2' C3' C4' 115.21(11) . . ? F4Z C4' F4Y 106.27(11) . . ? F4Z C4' F4X 106.27(11) . . ? F4Y C4' F4X 106.26(11) . . ? F4Z C4' C3' 110.1(17) . . ? F4Y C4' C3' 117.1(17) . . ? F4X C4' C3' 110.3(13) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.233 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.176 data_ilb1399_0m _database_code_depnum_ccdc_archive 'CCDC 903749' #TrackingRef 'SCSC2_step4_1-iPrOH_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H52 Ag4 F28 N6 O10' _chemical_formula_weight 1812.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9526(7) _cell_length_b 12.5368(9) _cell_length_c 15.4821(17) _cell_angle_alpha 109.945(7) _cell_angle_beta 97.373(7) _cell_angle_gamma 103.586(5) _cell_volume 1545.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 2716 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 20.65 _exptl_crystal_description 'block from a needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.947 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 890 _exptl_absorpt_coefficient_mu 1.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6969 _exptl_absorpt_correction_T_max 0.7053 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8043 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.1422 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3955 _reflns_number_gt 1865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3955 _refine_ls_number_parameters 406 _refine_ls_number_restraints 329 _refine_ls_R_factor_all 0.2309 _refine_ls_R_factor_gt 0.1384 _refine_ls_wR_factor_ref 0.4488 _refine_ls_wR_factor_gt 0.3574 _refine_ls_goodness_of_fit_ref 1.424 _refine_ls_restrained_S_all 2.595 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.1571(5) 0.5341(4) 0.8127(3) 0.0682(18) Uani 1 1 d . . . Ag2 Ag 0.5563(6) 0.4670(4) 0.3772(3) 0.080(2) Uani 1 1 d . . . N21 N 0.984(5) 0.511(3) 0.668(3) 0.054(5) Uani 1 1 d U . . N24 N 0.751(5) 0.484(3) 0.506(3) 0.057(5) Uani 1 1 d U . . C23 C 0.739(6) 0.392(4) 0.539(4) 0.056(5) Uani 1 1 d U . . C22 C 0.854(6) 0.408(4) 0.617(4) 0.055(5) Uani 1 1 d U . . C25 C 0.885(6) 0.588(4) 0.558(3) 0.057(5) Uani 1 1 d U . . C26 C 0.999(6) 0.595(4) 0.635(4) 0.055(5) Uani 1 1 d U . . C27 C 0.841(6) 0.305(4) 0.651(4) 0.056(8) Uani 1 1 d U . . H27A H 0.9289 0.3270 0.7039 0.084 Uiso 1 1 calc R . . H27B H 0.8440 0.2348 0.5999 0.084 Uiso 1 1 calc R . . H27C H 0.7427 0.2881 0.6706 0.084 Uiso 1 1 calc R . . C28 C 0.600(6) 0.285(4) 0.481(4) 0.062(8) Uani 1 1 d U . . H28A H 0.5405 0.3009 0.4328 0.093 Uiso 1 1 calc R . . H28B H 0.5323 0.2674 0.5222 0.093 Uiso 1 1 calc R . . H28C H 0.6367 0.2173 0.4524 0.093 Uiso 1 1 calc R . . C29 C 0.890(7) 0.681(4) 0.522(4) 0.062(8) Uani 1 1 d U . . H29A H 0.7990 0.6556 0.4703 0.092 Uiso 1 1 calc R . . H29B H 0.9858 0.6964 0.4993 0.092 Uiso 1 1 calc R . . H29C H 0.8890 0.7525 0.5719 0.092 Uiso 1 1 calc R . . C30 C 1.155(6) 0.709(4) 0.696(3) 0.060(8) Uani 1 1 d U . . H30A H 1.2149 0.6921 0.7433 0.090 Uiso 1 1 calc R . . H30B H 1.1212 0.7784 0.7262 0.090 Uiso 1 1 calc R . . H30C H 1.2200 0.7253 0.6536 0.090 Uiso 1 1 calc R . . N31 N 1.056(5) 0.518(3) 0.931(3) 0.056(7) Uani 1 1 d U . . C32 C 0.927(7) 0.541(4) 0.940(3) 0.058(7) Uani 1 1 d U . . C36 C 1.134(7) 0.471(4) 0.996(3) 0.056(7) Uani 1 1 d U . . C37 C 0.841(7) 0.584(5) 0.870(3) 0.061(9) Uani 1 1 d U . . H37A H 0.9023 0.5905 0.8241 0.092 Uiso 1 1 calc R . . H37B H 0.8295 0.6611 0.9052 0.092 Uiso 1 1 calc R . . H37C H 0.7376 0.5273 0.8386 0.092 Uiso 1 1 calc R . . C40 C 1.295(7) 0.452(5) 0.988(4) 0.065(9) Uani 1 1 d U . . H40A H 1.3238 0.4656 0.9334 0.098 Uiso 1 1 calc R . . H40B H 1.2892 0.3710 0.9805 0.098 Uiso 1 1 calc R . . H40C H 1.3733 0.5070 1.0445 0.098 Uiso 1 1 calc R . . O1S O 1.421(5) 0.686(3) 0.893(3) 0.107(11) Uani 1 1 d DU . . H1SO H 1.4912 0.6589 0.8663 0.161 Uiso 1 1 d RD . . C1S C 1.453(6) 0.795(5) 0.960(4) 0.111(11) Uani 1 1 d DU . . H1S H 1.4779 0.8391 0.9187 0.166 Uiso 1 1 calc R . . C2S C 1.296(7) 0.820(6) 0.971(5) 0.119(13) Uani 1 1 d DU . . H2S1 H 1.2138 0.7654 0.9160 0.179 Uiso 1 1 calc R . . H2S2 H 1.3049 0.9010 0.9778 0.179 Uiso 1 1 calc R . . H2S3 H 1.2690 0.8088 1.0270 0.179 Uiso 1 1 calc R . . C3S C 1.615(7) 0.851(6) 1.030(4) 0.114(13) Uani 1 1 d DU . . H3S1 H 1.6895 0.8123 1.0032 0.171 Uiso 1 1 calc R . . H3S2 H 1.6050 0.8420 1.0886 0.171 Uiso 1 1 calc R . . H3S3 H 1.6521 0.9352 1.0414 0.171 Uiso 1 1 calc R . . O1A O 0.430(6) 0.274(4) 0.229(3) 0.097(7) Uani 1 1 d U A . O1B O 0.270(5) 0.307(4) 0.310(3) 0.095(8) Uani 1 1 d U A . C1 C 0.295(6) 0.243(3) 0.243(4) 0.099(6) Uani 1 1 d DU . . C2 C 0.174(4) 0.120(2) 0.185(3) 0.102(6) Uiso 0.62(2) 1 d PDU A 1 C3 C 0.220(3) 0.024(3) 0.214(2) 0.105(6) Uiso 0.62(2) 1 d PDU A 1 F2A F 0.155(6) 0.090(5) 0.091(3) 0.101(8) Uiso 0.62(2) 1 d PDU A 1 F2B F 0.031(6) 0.117(5) 0.203(4) 0.105(8) Uiso 0.62(2) 1 d PDU A 1 F3B F 0.242(6) 0.064(5) 0.309(3) 0.107(8) Uiso 0.62(2) 1 d PDU A 1 F3A F 0.363(5) 0.022(5) 0.195(3) 0.105(8) Uiso 0.62(2) 1 d PDU A 1 C4 C 0.102(3) -0.101(2) 0.165(3) 0.107(6) Uiso 0.62(2) 1 d PDU A 1 F4A F 0.046(6) -0.140(5) 0.071(3) 0.107(8) Uiso 0.62(2) 1 d PDU A 1 F4B F -0.025(5) -0.115(5) 0.203(3) 0.112(8) Uiso 0.62(2) 1 d PDU A 1 F4C F 0.180(6) -0.175(5) 0.183(4) 0.110(8) Uiso 0.62(2) 1 d PDU A 1 C2' C 0.179(5) 0.120(2) 0.179(3) 0.102(6) Uiso 0.38(2) 1 d PDU A 2 C3' C 0.206(4) 0.028(3) 0.220(3) 0.105(6) Uiso 0.38(2) 1 d PDU A 2 C4' C 0.089(5) -0.098(3) 0.170(4) 0.107(6) Uiso 0.38(2) 1 d PDU A 2 F4X F 0.174(10) -0.151(8) 0.112(5) 0.110(8) Uiso 0.38(2) 1 d PDU A 2 F4Z F -0.064(5) -0.129(8) 0.125(6) 0.109(8) Uiso 0.38(2) 1 d PDU A 2 F4Y F 0.090(10) -0.140(8) 0.239(4) 0.108(8) Uiso 0.38(2) 1 d PDU A 2 F3Y F 0.093(6) 0.047(8) 0.268(6) 0.108(8) Uiso 0.38(2) 1 d PDU A 2 F3Z F 0.334(6) 0.041(9) 0.284(4) 0.106(8) Uiso 0.38(2) 1 d PDU A 2 F2Y F 0.034(5) 0.123(8) 0.147(6) 0.101(8) Uiso 0.38(2) 1 d PDU A 2 F2Z F 0.232(10) 0.069(9) 0.102(5) 0.104(9) Uiso 0.38(2) 1 d PDU A 2 O11A O 0.506(6) 0.614(5) 0.328(4) 0.119(8) Uani 1 1 d U B . O11B O 0.703(6) 0.589(5) 0.268(4) 0.121(8) Uani 1 1 d U . . C11 C 0.606(10) 0.643(4) 0.289(5) 0.123(7) Uani 1 1 d DU . . C12 C 0.623(4) 0.7572(18) 0.270(2) 0.126(7) Uiso 0.39(3) 1 d PDU B 1 F12A F 0.749(5) 0.759(10) 0.230(5) 0.125(9) Uiso 0.39(3) 1 d PDU B 1 F12B F 0.495(5) 0.723(11) 0.199(4) 0.124(9) Uiso 0.39(3) 1 d PDU B 1 C13 C 0.653(3) 0.886(2) 0.346(2) 0.130(7) Uiso 0.39(3) 1 d PDU B 1 C14 C 0.825(3) 0.933(3) 0.411(2) 0.133(8) Uiso 0.39(3) 1 d PDU B 1 F13A F 0.628(6) 0.963(2) 0.304(4) 0.133(9) Uiso 0.39(3) 1 d PDU B 1 F13B F 0.541(3) 0.887(5) 0.400(3) 0.131(10) Uiso 0.39(3) 1 d PDU B 1 F14A F 0.825(5) 1.019(5) 0.492(3) 0.137(10) Uiso 0.39(3) 1 d PDU B 1 F14B F 0.851(6) 0.843(4) 0.434(5) 0.133(9) Uiso 0.39(3) 1 d PDU B 1 F14C F 0.927(3) 0.953(7) 0.357(4) 0.135(10) Uiso 0.39(3) 1 d PDU B 1 C12' C 0.586(4) 0.7435(17) 0.2577(18) 0.126(7) Uiso 0.61(3) 1 d PDU B 2 F12Y F 0.655(5) 0.735(6) 0.184(3) 0.125(9) Uiso 0.61(3) 1 d PDU B 2 F12Z F 0.434(4) 0.733(7) 0.226(4) 0.122(9) Uiso 0.61(3) 1 d PDU B 2 C13' C 0.630(2) 0.8808(17) 0.3179(16) 0.130(7) Uiso 0.61(3) 1 d PDU B 2 F13Z F 0.655(4) 0.945(2) 0.262(2) 0.133(9) Uiso 0.61(3) 1 d PDU B 2 F13Y F 0.505(3) 0.910(3) 0.353(3) 0.135(9) Uiso 0.61(3) 1 d PDU B 2 C14' C 0.780(3) 0.921(2) 0.4004(16) 0.133(7) Uiso 0.61(3) 1 d PDU B 2 F14X F 0.889(3) 0.874(4) 0.363(3) 0.136(9) Uiso 0.61(3) 1 d PDU B 2 F14Y F 0.738(5) 0.868(4) 0.460(2) 0.131(10) Uiso 0.61(3) 1 d PDU B 2 F14Z F 0.812(5) 1.039(2) 0.449(3) 0.136(10) Uiso 0.61(3) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.074(4) 0.073(3) 0.064(3) 0.030(2) 0.019(2) 0.027(3) Ag2 0.097(4) 0.063(3) 0.073(3) 0.025(3) 0.005(3) 0.023(3) N21 0.066(12) 0.048(9) 0.062(11) 0.027(9) 0.025(9) 0.024(9) N24 0.067(12) 0.049(9) 0.064(11) 0.025(9) 0.025(9) 0.023(9) C23 0.066(12) 0.049(9) 0.063(11) 0.026(9) 0.026(9) 0.023(9) C22 0.066(12) 0.048(9) 0.062(11) 0.027(9) 0.026(9) 0.023(9) C25 0.067(12) 0.049(9) 0.064(11) 0.025(9) 0.025(9) 0.023(9) C26 0.066(12) 0.048(9) 0.063(11) 0.027(9) 0.025(9) 0.024(9) C27 0.068(16) 0.047(13) 0.064(15) 0.029(12) 0.025(13) 0.022(12) C28 0.069(16) 0.055(13) 0.066(15) 0.024(13) 0.026(13) 0.017(13) C29 0.068(16) 0.054(13) 0.067(15) 0.022(13) 0.022(13) 0.023(13) C30 0.068(16) 0.051(13) 0.067(15) 0.026(12) 0.024(13) 0.021(12) N31 0.078(19) 0.056(15) 0.053(14) 0.025(12) 0.037(13) 0.036(14) C32 0.079(19) 0.057(15) 0.054(15) 0.025(13) 0.036(14) 0.034(14) C36 0.079(19) 0.057(15) 0.052(15) 0.024(13) 0.037(14) 0.036(14) C37 0.08(2) 0.059(17) 0.059(17) 0.028(15) 0.033(16) 0.031(16) C40 0.09(2) 0.063(17) 0.058(17) 0.024(15) 0.033(16) 0.032(16) O1S 0.12(3) 0.065(19) 0.11(3) 0.003(17) 0.04(2) 0.02(2) C1S 0.12(3) 0.069(19) 0.11(3) 0.002(17) 0.04(2) 0.02(2) C2S 0.13(3) 0.07(2) 0.12(3) 0.00(2) 0.04(2) 0.01(2) C3S 0.13(3) 0.07(2) 0.11(3) 0.00(2) 0.03(2) 0.01(2) O1A 0.098(9) 0.098(8) 0.099(8) 0.042(7) 0.024(7) 0.032(7) O1B 0.093(12) 0.096(12) 0.100(12) 0.038(11) 0.024(11) 0.037(11) C1 0.100(7) 0.100(7) 0.101(7) 0.041(5) 0.024(4) 0.032(4) O11A 0.123(9) 0.121(9) 0.122(9) 0.053(7) 0.029(7) 0.043(7) O11B 0.124(9) 0.122(9) 0.124(9) 0.051(7) 0.028(7) 0.044(7) C11 0.125(8) 0.124(8) 0.124(8) 0.050(5) 0.029(4) 0.041(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N31 2.20(4) . ? Ag1 O11B 2.34(5) 2_766 ? Ag1 N21 2.45(4) . ? Ag1 O1S 2.50(5) . ? Ag2 O11A 2.33(5) . ? Ag2 N24 2.39(4) . ? Ag2 O1A 2.59(5) . ? N21 C26 1.30(5) . ? N21 C22 1.41(6) . ? N24 C23 1.40(6) . ? N24 C25 1.44(6) . ? C23 C22 1.41(7) . ? C23 C28 1.50(7) . ? C22 C27 1.54(6) . ? C25 C26 1.44(7) . ? C25 C29 1.44(6) . ? C26 C30 1.64(7) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? N31 C32 1.26(6) . ? N31 C36 1.51(6) . ? C32 C36 1.23(6) 2_767 ? C32 C37 1.56(7) . ? C36 C32 1.23(6) 2_767 ? C36 C40 1.53(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 H40C 0.9700 . ? O1S C1S 1.34(3) . ? O1S H1SO 0.8700 . ? C1S C2S 1.532(19) . ? C1S C3S 1.534(19) . ? C1S H1S 0.9900 . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C2S H2S3 0.9700 . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C3S H3S3 0.9700 . ? O1A C1 1.24(6) . ? O1B C1 1.17(6) . ? C1 C2 1.5399(19) . ? C1 C2' 1.5401(19) . ? C2 F2A 1.3500(19) . ? C2 F2B 1.3500(19) . ? C2 C3 1.5401(19) . ? C3 F3A 1.3500(19) . ? C3 F3B 1.3501(19) . ? C3 C4 1.5400(19) . ? C4 F4C 1.3499(19) . ? C4 F4B 1.3499(19) . ? C4 F4A 1.3500(19) . ? C2' F2Z 1.3500(19) . ? C2' F2Y 1.3501(19) . ? C2' C3' 1.5400(19) . ? C3' F3Z 1.3500(19) . ? C3' F3Y 1.3500(19) . ? C3' C4' 1.5400(19) . ? C4' F4Z 1.3500(19) . ? C4' F4X 1.3500(19) . ? C4' F4Y 1.3500(19) . ? O11A C11 1.19(8) . ? O11B C11 1.24(8) . ? O11B Ag1 2.34(5) 2_766 ? C11 C12' 1.5400(19) . ? C11 C12 1.5401(19) . ? C12 F12A 1.350(2) . ? C12 F12B 1.350(2) . ? C12 C13 1.5737(17) . ? C13 F13B 1.3805(18) . ? C13 F13A 1.3805(17) . ? C13 C14 1.5736(17) . ? C14 F14C 1.350(2) . ? C14 F14B 1.3499(19) . ? C14 F14A 1.3500(19) . ? C12' F12Y 1.350(2) . ? C12' F12Z 1.3500(19) . ? C12' C13' 1.5736(17) . ? C13' F13Z 1.3805(18) . ? C13' F13Y 1.3805(17) . ? C13' C14' 1.5738(17) . ? C14' F14Y 1.3501(19) . ? C14' F14X 1.350(2) . ? C14' F14Z 1.350(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 N31 Ag1 O11B 124.8(15) . 2_766 ? N31 Ag1 N21 119.6(15) . . ? O11B Ag1 N21 93.7(16) 2_766 . ? N31 Ag1 O1S 103.0(16) . . ? O11B Ag1 O1S 86.1(16) 2_766 . ? N21 Ag1 O1S 126.7(15) . . ? O11A Ag2 N24 129.6(16) . . ? O11A Ag2 O1A 103.5(16) . . ? N24 Ag2 O1A 123.5(13) . . ? C26 N21 C22 116(4) . . ? C26 N21 Ag1 122(3) . . ? C22 N21 Ag1 122(3) . . ? C23 N24 C25 115(4) . . ? C23 N24 Ag2 121(3) . . ? C25 N24 Ag2 124(3) . . ? N24 C23 C22 119(5) . . ? N24 C23 C28 113(4) . . ? C22 C23 C28 129(4) . . ? N21 C22 C23 126(4) . . ? N21 C22 C27 116(4) . . ? C23 C22 C27 118(5) . . ? N24 C25 C26 122(4) . . ? N24 C25 C29 113(4) . . ? C26 C25 C29 125(5) . . ? N21 C26 C25 122(5) . . ? N21 C26 C30 113(4) . . ? C25 C26 C30 125(4) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 N31 C36 121(4) . . ? C32 N31 Ag1 120(3) . . ? C36 N31 Ag1 119(3) . . ? C36 C32 N31 121(5) 2_767 . ? C36 C32 C37 118(5) 2_767 . ? N31 C32 C37 121(4) . . ? C32 C36 C40 121(5) 2_767 . ? C32 C36 N31 118(4) 2_767 . ? C40 C36 N31 120(4) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1S O1S Ag1 128(3) . . ? C1S O1S H1SO 123.4 . . ? Ag1 O1S H1SO 108.0 . . ? C2S C1S C3S 130(5) . . ? C2S C1S O1S 107(5) . . ? C3S C1S O1S 119(4) . . ? C2S C1S H1S 96.4 . . ? C3S C1S H1S 96.4 . . ? O1S C1S H1S 96.4 . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C1S C3S H3S1 109.5 . . ? C1S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C1S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 109.5 . . ? C1 O1A Ag2 100(3) . . ? O1B C1 O1A 116(4) . . ? O1B C1 C2 120(5) . . ? O1A C1 C2 123(5) . . ? O1B C1 C2' 123(5) . . ? O1A C1 C2' 120(5) . . ? F2A C2 F2B 106.3(2) . . ? F2A C2 C1 113(4) . . ? F2B C2 C1 111(4) . . ? F2A C2 C3 111(4) . . ? F2B C2 C3 104(4) . . ? C1 C2 C3 110(3) . . ? F3A C3 F3B 106.2(2) . . ? F3A C3 C2 107(4) . . ? F3B C3 C2 107(4) . . ? F3A C3 C4 109(4) . . ? F3B C3 C4 112(4) . . ? C2 C3 C4 115.2(2) . . ? F4C C4 F4B 106.3(2) . . ? F4C C4 F4A 109(4) . . ? F4B C4 F4A 106.3(2) . . ? F4C C4 C3 105(3) . . ? F4B C4 C3 113(4) . . ? F4A C4 C3 117(3) . . ? F2Z C2' F2Y 106.2(2) . . ? F2Z C2' C3' 92(5) . . ? F2Y C2' C3' 123(5) . . ? F2Z C2' C1 111(6) . . ? F2Y C2' C1 114(5) . . ? C3' C2' C1 109(3) . . ? F3Z C3' F3Y 106.3(2) . . ? F3Z C3' C4' 117(5) . . ? F3Y C3' C4' 83(5) . . ? F3Z C3' C2' 127(5) . . ? F3Y C3' C2' 89(5) . . ? C4' C3' C2' 115.2(2) . . ? F4Z C4' F4X 112(6) . . ? F4Z C4' F4Y 106.3(2) . . ? F4X C4' F4Y 106.3(2) . . ? F4Z C4' C3' 129(5) . . ? F4X C4' C3' 100(5) . . ? F4Y C4' C3' 102(5) . . ? C11 O11A Ag2 109(4) . . ? C11 O11B Ag1 165(5) . 2_766 ? O11A C11 O11B 123(4) . . ? O11A C11 C12' 113(6) . . ? O11B C11 C12' 123(6) . . ? O11A C11 C12 120(6) . . ? O11B C11 C12 117(6) . . ? F12A C12 F12B 106.3(2) . . ? F12A C12 C11 100(6) . . ? F12B C12 C11 101(6) . . ? F12A C12 C13 107(5) . . ? F12B C12 C13 113(5) . . ? C11 C12 C13 126(4) . . ? F13B C13 F13A 102.15(16) . . ? F13B C13 C12 110.97(16) . . ? F13A C13 C12 110.98(16) . . ? F13B C13 C14 110.98(16) . . ? F13A C13 C14 110.98(17) . . ? C12 C13 C14 110.53(15) . . ? F14C C14 F14B 106.3(2) . . ? F14C C14 F14A 121.4(5) . . ? F14B C14 F14A 106.3(2) . . ? F14C C14 C13 107.41(19) . . ? F14B C14 C13 107.41(19) . . ? F14A C14 C13 107.41(19) . . ? F12Y C12' F12Z 106.3(2) . . ? F12Y C12' C11 107(5) . . ? F12Z C12' C11 113(5) . . ? F12Y C12' C13' 105(3) . . ? F12Z C12' C13' 94(3) . . ? C11 C12' C13' 129(3) . . ? F13Z C13' F13Y 102.15(16) . . ? F13Z C13' C12' 110.99(16) . . ? F13Y C13' C12' 110.99(16) . . ? F13Z C13' C14' 110.97(17) . . ? F13Y C13' C14' 110.97(16) . . ? C12' C13' C14' 110.52(15) . . ? F14Y C14' F14X 106.2(2) . . ? F14Y C14' F14Z 106.3(2) . . ? F14X C14' F14Z 121.5(5) . . ? F14Y C14' C13' 107.38(19) . . ? F14X C14' C13' 107.39(19) . . ? F14Z C14' C13' 107.38(19) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 2.611 _refine_diff_density_min -1.369 _refine_diff_density_rms 0.305 data_ilb1406_0m _database_code_depnum_ccdc_archive 'CCDC 903750' #TrackingRef 'SCSC2_step5_1_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 Ag4 F28 N6 O8' _chemical_formula_weight 1692.23 _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5195(5) _cell_length_b 12.9328(7) _cell_length_c 15.4193(10) _cell_angle_alpha 106.412(4) _cell_angle_beta 105.705(4) _cell_angle_gamma 109.208(4) _cell_volume 1409.52(14) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 5574 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 25.83 _exptl_crystal_description 'BLOCK FROM A NEEDLE' _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.994 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 1.514 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6765 _exptl_absorpt_correction_T_max 0.6853 _exptl_absorpt_process_details SADABAS _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21785 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.1187 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6438 _reflns_number_gt 2760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6438 _refine_ls_number_parameters 376 _refine_ls_number_restraints 289 _refine_ls_R_factor_all 0.2389 _refine_ls_R_factor_gt 0.1306 _refine_ls_wR_factor_ref 0.3622 _refine_ls_wR_factor_gt 0.3268 _refine_ls_goodness_of_fit_ref 1.775 _refine_ls_restrained_S_all 1.764 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.36465(17) 0.72160(12) 1.29269(10) 0.0655(5) Uani 1 1 d . . . Ag2 Ag 0.48417(18) 0.39085(12) 0.87619(10) 0.0676(5) Uani 1 1 d . . . N21 N 1.0783(16) 0.6230(11) 1.1710(9) 0.0471(19) Uani 1 1 d U . . C23 C 0.8003(19) 0.4482(13) 1.0718(11) 0.0477(19) Uani 1 1 d U . . C22 C 0.9697(19) 0.5143(13) 1.1515(11) 0.0468(19) Uani 1 1 d U . . N24 N 0.7500(15) 0.4987(11) 1.0141(9) 0.0465(19) Uani 1 1 d U . . C25 C 0.857(2) 0.6107(14) 1.0279(11) 0.050(2) Uani 1 1 d U . . C26 C 1.028(2) 0.6753(13) 1.1110(11) 0.050(2) Uani 1 1 d U . . C28 C 0.675(2) 0.3329(14) 1.0558(12) 0.059(3) Uani 1 1 d U . . H28A H 0.5611 0.3090 1.0042 0.089 Uiso 1 1 calc R . . H28B H 0.6590 0.3360 1.1155 0.089 Uiso 1 1 calc R . . H28C H 0.7221 0.2758 1.0370 0.089 Uiso 1 1 calc R . . C27 C 1.034(2) 0.4633(14) 1.2225(12) 0.053(3) Uani 1 1 d U . . H27A H 1.1574 0.5168 1.2673 0.079 Uiso 1 1 calc R . . H27B H 1.0261 0.3867 1.1865 0.079 Uiso 1 1 calc R . . H27C H 0.9589 0.4539 1.2590 0.079 Uiso 1 1 calc R . . C29 C 0.791(2) 0.6687(16) 0.9614(12) 0.063(3) Uani 1 1 d U . . H29A H 0.6715 0.6133 0.9122 0.095 Uiso 1 1 calc R . . H29B H 0.8723 0.6892 0.9297 0.095 Uiso 1 1 calc R . . H29C H 0.7883 0.7399 1.0004 0.095 Uiso 1 1 calc R . . C30 C 1.148(2) 0.8037(14) 1.1329(13) 0.061(3) Uani 1 1 d U . . H30A H 1.2678 0.8281 1.1792 0.092 Uiso 1 1 calc R . . H30B H 1.0981 0.8551 1.1604 0.092 Uiso 1 1 calc R . . H30C H 1.1528 0.8094 1.0729 0.092 Uiso 1 1 calc R . . N31 N 1.4468(16) 0.8844(11) 1.4338(9) 0.049(2) Uani 1 1 d U . . C32 C 1.3234(19) 0.9253(14) 1.4487(11) 0.050(2) Uani 1 1 d U . . C36 C 1.6180(19) 0.9613(14) 1.4861(11) 0.050(2) Uani 1 1 d U . . C37 C 1.1291(19) 0.8407(15) 1.3949(12) 0.058(3) Uani 1 1 d U . . H37A H 1.1158 0.7599 1.3762 0.086 Uiso 1 1 calc R . . H37B H 1.0791 0.8526 1.3369 0.086 Uiso 1 1 calc R . . H37C H 1.0661 0.8545 1.4368 0.086 Uiso 1 1 calc R . . C40 C 1.746(2) 0.9082(15) 1.4749(12) 0.056(3) Uani 1 1 d U . . H40A H 1.6992 0.8292 1.4738 0.084 Uiso 1 1 calc R . . H40B H 1.8620 0.9578 1.5294 0.084 Uiso 1 1 calc R . . H40C H 1.7598 0.9034 1.4143 0.084 Uiso 1 1 calc R . . O1A O 0.242(2) 0.1965(14) 0.8288(11) 0.092(3) Uani 1 1 d U A . O1B O 0.433(2) 0.1613(14) 0.7723(11) 0.097(3) Uani 1 1 d U . . C1 C 0.292(3) 0.1331(11) 0.7879(17) 0.100(2) Uani 1 1 d DU . . F2A F 0.148(2) -0.0714(16) 0.6587(11) 0.106(3) Uiso 0.699(10) 1 d PDU A 1 C2 C 0.1601(17) -0.0007(10) 0.7459(8) 0.106(2) Uiso 0.699(10) 1 d PDU A 1 F4C F 0.186(2) -0.1116(14) 0.9462(14) 0.118(4) Uiso 0.699(10) 1 d PDU A 1 C3 C 0.212(2) -0.0655(11) 0.8107(10) 0.112(2) Uiso 0.699(10) 1 d PDU A 1 F4A F 0.3107(19) 0.0850(14) 0.9742(13) 0.118(4) Uiso 0.699(10) 1 d PDU A 1 F3A F 0.3850(17) -0.0500(15) 0.8439(15) 0.122(4) Uiso 0.699(10) 1 d PDU A 1 F2B F -0.012(2) -0.0220(18) 0.7352(12) 0.103(4) Uiso 0.699(10) 1 d PDU A 1 F3B F 0.1066(19) -0.1851(12) 0.7662(14) 0.115(3) Uiso 0.699(10) 1 d PDU A 1 F4B F 0.0247(17) -0.0297(15) 0.8873(14) 0.129(4) Uiso 0.699(10) 1 d PDU A 1 C4 C 0.1902(18) -0.0281(12) 0.9094(10) 0.115(3) Uiso 0.699(10) 1 d PDU A 1 C2' C 0.178(3) -0.0034(11) 0.7476(13) 0.107(2) Uiso 0.301(10) 1 d PDU A 2 C3' C 0.108(2) -0.0663(19) 0.8100(17) 0.112(2) Uiso 0.301(10) 1 d PDU A 2 F2Z F 0.240(3) -0.060(3) 0.688(2) 0.108(4) Uiso 0.301(10) 1 d PDU A 2 F2Y F 0.001(3) -0.039(4) 0.693(2) 0.103(4) Uiso 0.301(10) 1 d PDU A 2 F4Z F 0.420(3) 0.044(3) 0.928(3) 0.119(4) Uiso 0.301(10) 1 d PDU A 2 F4X F 0.277(5) -0.070(3) 0.984(2) 0.115(4) Uiso 0.301(10) 1 d PDU A 2 F4Y F 0.174(4) 0.047(3) 0.940(3) 0.119(4) Uiso 0.301(10) 1 d PDU A 2 C4' C 0.250(3) -0.027(2) 0.9139(15) 0.115(3) Uiso 0.301(10) 1 d PDU A 2 F3Z F 0.276(2) -0.062(4) 0.838(3) 0.117(3) Uiso 0.301(10) 1 d PDU A 2 F3Y F -0.007(4) -0.177(2) 0.795(3) 0.117(5) Uiso 0.301(10) 1 d PDU A 2 O11A O 0.331(2) 0.4478(14) 0.7645(12) 0.099(3) Uani 1 1 d U B . O11B O 0.499(2) 0.4053(14) 0.6897(11) 0.097(3) Uani 1 1 d U . . C11 C 0.394(3) 0.445(2) 0.6994(15) 0.103(2) Uani 1 1 d DU . . C12 C 0.3123(15) 0.4855(9) 0.6209(9) 0.111(2) Uiso 0.678(11) 1 d PDU B 1 C13 C 0.4359(12) 0.6184(9) 0.6509(8) 0.119(2) Uiso 0.678(11) 1 d PDU B 1 C14 C 0.3579(13) 0.6775(8) 0.5880(8) 0.127(3) Uiso 0.678(11) 1 d PDU B 1 F12A F 0.154(2) 0.4877(18) 0.6178(13) 0.109(4) Uiso 0.678(11) 1 d PDU B 1 F13A F 0.496(2) 0.6856(18) 0.7482(9) 0.121(4) Uiso 0.678(11) 1 d PDU B 1 F14A F 0.1987(16) 0.6698(15) 0.5927(13) 0.148(5) Uiso 0.678(11) 1 d PDU B 1 F12B F 0.279(3) 0.4096(18) 0.5304(12) 0.115(4) Uiso 0.678(11) 1 d PDU B 1 F14B F 0.319(2) 0.6154(13) 0.4924(7) 0.133(4) Uiso 0.678(11) 1 d PDU B 1 F13B F 0.581(2) 0.6101(18) 0.6356(12) 0.119(4) Uiso 0.678(11) 1 d PDU B 1 F14C F 0.4858(19) 0.7889(9) 0.6145(13) 0.134(4) Uiso 0.678(11) 1 d PDU B 1 C12' C 0.335(2) 0.5025(12) 0.6297(13) 0.112(2) Uiso 0.322(11) 1 d PDU B 2 C13' C 0.476(2) 0.6346(12) 0.6764(10) 0.119(3) Uiso 0.322(11) 1 d PDU B 2 F13Z F 0.399(3) 0.684(3) 0.731(2) 0.119(4) Uiso 0.322(11) 1 d PDU B 2 F13Y F 0.6573(19) 0.695(3) 0.730(2) 0.123(4) Uiso 0.322(11) 1 d PDU B 2 F12Z F 0.152(2) 0.449(4) 0.593(3) 0.111(4) Uiso 0.322(11) 1 d PDU B 2 F12Y F 0.379(5) 0.474(4) 0.552(2) 0.113(4) Uiso 0.322(11) 1 d PDU B 2 F14Y F 0.452(3) 0.658(2) 0.5277(14) 0.130(4) Uiso 0.322(11) 1 d PDU B 2 F14X F 0.583(3) 0.8195(12) 0.662(2) 0.132(5) Uiso 0.322(11) 1 d PDU B 2 F14Z F 0.277(3) 0.700(2) 0.595(2) 0.135(4) Uiso 0.322(11) 1 d PDU B 2 C14' C 0.446(2) 0.7075(11) 0.6155(14) 0.125(3) Uiso 0.322(11) 1 d PDU B 2 _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 0.0498(8) 0.0592(9) 0.0714(10) 0.0162(7) 0.0127(6) 0.0239(6) Ag2 0.0592(9) 0.0642(10) 0.0643(9) 0.0244(7) 0.0134(7) 0.0208(7) N21 0.046(3) 0.049(3) 0.055(4) 0.023(3) 0.027(3) 0.023(3) C23 0.046(3) 0.050(3) 0.055(4) 0.024(3) 0.025(3) 0.023(3) C22 0.045(3) 0.050(3) 0.055(4) 0.023(3) 0.026(3) 0.024(3) N24 0.044(3) 0.049(3) 0.054(4) 0.024(3) 0.023(3) 0.024(3) C25 0.047(3) 0.050(3) 0.056(4) 0.023(3) 0.024(3) 0.023(3) C26 0.047(3) 0.049(3) 0.057(4) 0.023(3) 0.024(3) 0.023(3) C28 0.058(6) 0.050(5) 0.061(6) 0.024(5) 0.016(5) 0.019(5) C27 0.052(5) 0.054(5) 0.060(6) 0.028(5) 0.026(5) 0.024(5) C29 0.055(5) 0.061(6) 0.063(6) 0.020(5) 0.017(5) 0.023(5) C30 0.056(6) 0.054(6) 0.065(6) 0.027(5) 0.012(5) 0.022(5) N31 0.044(4) 0.060(5) 0.053(5) 0.024(4) 0.023(4) 0.031(4) C32 0.043(4) 0.060(5) 0.054(5) 0.024(4) 0.021(4) 0.030(4) C36 0.045(4) 0.061(5) 0.052(5) 0.021(4) 0.026(4) 0.030(4) C37 0.044(5) 0.063(6) 0.060(6) 0.017(5) 0.017(5) 0.027(5) C40 0.045(5) 0.063(6) 0.063(6) 0.015(5) 0.023(5) 0.034(5) O1A 0.097(4) 0.099(4) 0.101(4) 0.048(3) 0.049(3) 0.052(3) O1B 0.096(4) 0.104(4) 0.105(4) 0.047(3) 0.048(3) 0.051(3) C1 0.101(3) 0.103(3) 0.104(3) 0.046(2) 0.046(2) 0.049(2) O11A 0.105(4) 0.103(4) 0.108(4) 0.055(3) 0.042(3) 0.058(3) O11B 0.100(4) 0.103(4) 0.112(4) 0.052(3) 0.044(3) 0.065(3) C11 0.106(3) 0.106(3) 0.110(3) 0.050(2) 0.044(2) 0.057(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _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 N21 2.285(12) . ? Ag1 N31 2.297(12) . ? Ag1 O11B 2.335(14) 2_767 ? Ag1 O1B 2.520(16) 2_767 ? Ag2 N24 2.288(12) . ? Ag2 O11A 2.310(14) . ? Ag2 O1A 2.418(15) . ? N21 C22 1.295(19) . ? N21 C26 1.350(19) . ? C23 N24 1.307(18) . ? C23 C22 1.40(2) . ? C23 C28 1.42(2) . ? C22 C27 1.50(2) . ? N24 C25 1.352(19) . ? C25 C26 1.43(2) . ? C25 C29 1.53(2) . ? C26 C30 1.51(2) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N31 C36 1.313(19) . ? N31 C32 1.365(18) . ? C32 C36 1.35(2) 2_878 ? C32 C37 1.48(2) . ? C36 C32 1.35(2) 2_878 ? C36 C40 1.491(19) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? O1A C1 1.16(2) . ? O1B C1 1.24(2) . ? O1B Ag1 2.520(16) 2_767 ? C1 C2' 1.5400(11) . ? C1 C2 1.5400(11) . ? F2A C2 1.3499(10) . ? C2 F2B 1.3500(10) . ? C2 C3 1.5400(10) . ? F4C C4 1.3500(10) . ? C3 F3A 1.3500(10) . ? C3 F3B 1.3500(11) . ? C3 C4 1.5400(10) . ? F4A C4 1.3500(11) . ? F4B C4 1.3499(10) . ? C2' F2Z 1.3500(10) . ? C2' F2Y 1.3500(11) . ? C2' C3' 1.5400(10) . ? C3' F3Y 1.3500(11) . ? C3' F3Z 1.3501(11) . ? C3' C4' 1.5399(11) . ? F4Z C4' 1.3500(11) . ? F4X C4' 1.3499(10) . ? F4Y C4' 1.3500(10) . ? O11A C11 1.26(2) . ? O11B C11 1.19(2) . ? O11B Ag1 2.335(14) 2_767 ? C11 C12 1.5398(10) . ? C11 C12' 1.5403(10) . ? C12 F12B 1.3500(10) . ? C12 F12A 1.3500(10) . ? C12 C13 1.5400(11) . ? C13 F13A 1.3500(10) . ? C13 F13B 1.3501(10) . ? C13 C14 1.5402(10) . ? C14 F14C 1.3498(11) . ? C14 F14B 1.3499(10) . ? C14 F14A 1.3500(10) . ? C12' F12Y 1.3500(10) . ? C12' F12Z 1.3501(11) . ? C12' C13' 1.5398(11) . ? C13' F13Y 1.3499(12) . ? C13' F13Z 1.3499(10) . ? C13' C14' 1.5394(10) . ? F14Y C14' 1.3496(10) . ? F14X C14' 1.3499(11) . ? F14Z C14' 1.3496(10) . ? _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 N21 Ag1 N31 122.2(4) . . ? N21 Ag1 O11B 113.0(5) . 2_767 ? N31 Ag1 O11B 116.2(5) . 2_767 ? N21 Ag1 O1B 106.8(5) . 2_767 ? N31 Ag1 O1B 94.9(5) . 2_767 ? O11B Ag1 O1B 97.8(5) 2_767 2_767 ? N24 Ag2 O11A 131.4(5) . . ? N24 Ag2 O1A 129.0(5) . . ? O11A Ag2 O1A 97.9(5) . . ? C22 N21 C26 118.9(13) . . ? C22 N21 Ag1 122.1(10) . . ? C26 N21 Ag1 118.5(10) . . ? N24 C23 C22 118.2(14) . . ? N24 C23 C28 118.8(14) . . ? C22 C23 C28 122.8(14) . . ? N21 C22 C23 123.2(14) . . ? N21 C22 C27 115.7(13) . . ? C23 C22 C27 121.1(14) . . ? C23 N24 C25 122.2(13) . . ? C23 N24 Ag2 119.9(10) . . ? C25 N24 Ag2 117.6(9) . . ? N24 C25 C26 117.5(13) . . ? N24 C25 C29 120.8(13) . . ? C26 C25 C29 121.6(14) . . ? N21 C26 C25 119.9(14) . . ? N21 C26 C30 120.9(13) . . ? C25 C26 C30 119.2(13) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 N31 C32 115.7(13) . . ? C36 N31 Ag1 120.4(10) . . ? C32 N31 Ag1 120.6(10) . . ? N31 C32 C36 119.6(14) . 2_878 ? N31 C32 C37 117.9(14) . . ? C36 C32 C37 122.4(14) 2_878 . ? N31 C36 C32 124.6(13) . 2_878 ? N31 C36 C40 113.4(14) . . ? C32 C36 C40 121.7(14) 2_878 . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1 O1A Ag2 101.3(11) . . ? C1 O1B Ag1 149.6(14) . 2_767 ? O1A C1 O1B 127.7(14) . . ? O1A C1 C2' 119(2) . . ? O1B C1 C2' 114(2) . . ? O1A C1 C2 113.5(19) . . ? O1B C1 C2 118.8(19) . . ? F2A C2 F2B 106.25(11) . . ? F2A C2 C3 100.9(12) . . ? F2B C2 C3 103.5(12) . . ? F2A C2 C1 116.2(15) . . ? F2B C2 C1 114.4(16) . . ? C3 C2 C1 114.0(13) . . ? F3A C3 F3B 106.26(11) . . ? F3A C3 C2 117.9(13) . . ? F3B C3 C2 112.4(13) . . ? F3A C3 C4 99.9(13) . . ? F3B C3 C4 103.5(14) . . ? C2 C3 C4 115.16(11) . . ? F4B C4 F4C 106.27(11) . . ? F4B C4 F4A 106.26(11) . . ? F4C C4 F4A 114.1(16) . . ? F4B C4 C3 106.0(13) . . ? F4C C4 C3 110.1(13) . . ? F4A C4 C3 113.4(12) . . ? F2Z C2' F2Y 106.26(11) . . ? F2Z C2' C3' 116(3) . . ? F2Y C2' C3' 86(2) . . ? F2Z C2' C1 109(2) . . ? F2Y C2' C1 113(3) . . ? C3' C2' C1 123.3(16) . . ? F3Y C3' F3Z 106.25(11) . . ? F3Y C3' C4' 100(2) . . ? F3Z C3' C4' 50(2) . . ? F3Y C3' C2' 137(3) . . ? F3Z C3' C2' 82(2) . . ? C4' C3' C2' 115.17(11) . . ? F4X C4' F4Y 106.27(11) . . ? F4X C4' F4Z 104(3) . . ? F4Y C4' F4Z 106.27(11) . . ? F4X C4' C3' 138(2) . . ? F4Y C4' C3' 83(3) . . ? F4Z C4' C3' 112.9(19) . . ? C11 O11A Ag2 109.0(10) . . ? C11 O11B Ag1 152.7(14) . 2_767 ? O11B C11 O11A 125.4(12) . . ? O11B C11 C12 118.5(19) . . ? O11A C11 C12 115.8(18) . . ? O11B C11 C12' 118(2) . . ? O11A C11 C12' 116(2) . . ? F12B C12 F12A 106.98(11) . . ? F12B C12 C11 109.9(16) . . ? F12A C12 C11 113.3(17) . . ? F12B C12 C13 115.4(14) . . ? F12A C12 C13 102.2(12) . . ? C11 C12 C13 109.0(11) . . ? F13A C13 F13B 106.25(11) . . ? F13A C13 C12 112.8(13) . . ? F13B C13 C12 100.7(13) . . ? F13A C13 C14 111.3(12) . . ? F13B C13 C14 109.8(11) . . ? C12 C13 C14 115.14(11) . . ? F14C C14 F14B 106.28(11) . . ? F14C C14 F14A 116.1(3) . . ? F14B C14 F14A 106.27(11) . . ? F14C C14 C13 109.32(11) . . ? F14B C14 C13 109.30(11) . . ? F14A C14 C13 109.31(11) . . ? F12Y C12' F12Z 106.25(12) . . ? F12Y C12' C13' 94(2) . . ? F12Z C12' C13' 133(3) . . ? F12Y C12' C11 111(3) . . ? F12Z C12' C11 104(2) . . ? C13' C12' C11 107.0(12) . . ? F13Y C13' F13Z 106.27(11) . . ? F13Y C13' C14' 101(2) . . ? F13Z C13' C14' 88(2) . . ? F13Y C13' C12' 136(2) . . ? F13Z C13' C12' 99(2) . . ? C14' C13' C12' 115.24(11) . . ? F14Z C14' F14Y 106.31(11) . . ? F14Z C14' F14X 115.9(3) . . ? F14Y C14' F14X 106.30(11) . . ? F14Z C14' C13' 109.39(11) . . ? F14Y C14' C13' 109.39(11) . . ? F14X C14' C13' 109.37(11) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.281 _refine_diff_density_min -1.417 _refine_diff_density_rms 0.288 data_ilb1421_0m _database_code_depnum_ccdc_archive 'CCDC 903751' #TrackingRef 'SCSC2_step6(end)_1-EtOH_240K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 Ag4 F28 N6 O10' _chemical_formula_weight 1784.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8900(13) _cell_length_b 12.5176(15) _cell_length_c 15.367(3) _cell_angle_alpha 110.116(13) _cell_angle_beta 97.006(14) _cell_angle_gamma 104.064(9) _cell_volume 1517.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 5314 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 26.40 _exptl_crystal_description 'block from a needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.953 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 1.414 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6928 _exptl_absorpt_correction_T_max 0.7100 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15876 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3927 _reflns_number_gt 2194 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3927 _refine_ls_number_parameters 379 _refine_ls_number_restraints 299 _refine_ls_R_factor_all 0.2484 _refine_ls_R_factor_gt 0.1680 _refine_ls_wR_factor_ref 0.4430 _refine_ls_wR_factor_gt 0.3746 _refine_ls_goodness_of_fit_ref 2.597 _refine_ls_restrained_S_all 2.806 _refine_ls_shift/su_max 0.190 _refine_ls_shift/su_mean 0.026 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.1500(3) 0.77931(19) 0.81253(16) 0.0768(10) Uani 1 1 d . . . Ag2 Ag 0.3200(4) 0.4064(2) 0.37453(18) 0.0884(12) Uani 1 1 d . . . N21 N 0.180(3) 0.6572(16) 0.6672(15) 0.061(3) Uani 1 1 d U C . N24 N 0.256(3) 0.5210(16) 0.5057(15) 0.059(3) Uani 1 1 d U . . C23 C 0.300(3) 0.643(2) 0.5344(19) 0.060(3) Uani 1 1 d U C . C22 C 0.255(3) 0.710(2) 0.6157(19) 0.060(3) Uani 1 1 d U . . C26 C 0.143(3) 0.542(2) 0.6412(19) 0.059(3) Uani 1 1 d U . . C25 C 0.182(3) 0.474(2) 0.5610(19) 0.059(3) Uani 1 1 d U C . C27 C 0.307(4) 0.844(2) 0.651(2) 0.065(5) Uani 1 1 d U C . H27A H 0.2282 0.8742 0.6800 0.098 Uiso 1 1 calc R . . H27B H 0.3200 0.8677 0.5984 0.098 Uiso 1 1 calc R . . H27C H 0.4066 0.8762 0.6968 0.098 Uiso 1 1 calc R . . C30 C 0.135(4) 0.335(2) 0.5250(19) 0.065(5) Uani 1 1 d U . . H30A H 0.0386 0.3006 0.4765 0.097 Uiso 1 1 calc R C . H30B H 0.1191 0.3114 0.5770 0.097 Uiso 1 1 calc R . . H30C H 0.2187 0.3087 0.4993 0.097 Uiso 1 1 calc R . . C28 C 0.391(4) 0.699(2) 0.4798(19) 0.063(4) Uani 1 1 d U . . H28A H 0.4997 0.7389 0.5149 0.095 Uiso 1 1 calc R C . H28B H 0.3453 0.7567 0.4688 0.095 Uiso 1 1 calc R . . H28C H 0.3887 0.6394 0.4199 0.095 Uiso 1 1 calc R . . C29 C 0.055(4) 0.482(2) 0.7029(19) 0.063(4) Uani 1 1 d U C . H29A H 0.1006 0.5299 0.7691 0.094 Uiso 1 1 calc R . . H29B H 0.0655 0.4037 0.6880 0.094 Uiso 1 1 calc R . . H29C H -0.0560 0.4761 0.6892 0.094 Uiso 1 1 calc R . . O1S O -0.038(3) 0.7189(18) 0.8957(15) 0.099(6) Uani 1 1 d DU A . C1S C -0.017(4) 0.708(5) 0.985(2) 0.101(6) Uiso 0.65(4) 1 d PDU A 1 H1S1 H -0.1125 0.6543 0.9883 0.121 Uiso 0.65(4) 1 calc PR A 1 H1S2 H 0.0050 0.7856 1.0357 0.121 Uiso 0.65(4) 1 calc PR A 1 C2S C 0.124(5) 0.659(5) 0.992(4) 0.104(7) Uiso 0.65(4) 1 d PDU A 1 H2S1 H 0.1249 0.6044 0.9308 0.156 Uiso 0.65(4) 1 calc PR A 1 H2S2 H 0.1145 0.6178 1.0349 0.156 Uiso 0.65(4) 1 calc PR A 1 H2S3 H 0.2221 0.7237 1.0167 0.156 Uiso 0.65(4) 1 calc PR A 1 C1S' C 0.001(7) 0.674(7) 0.965(4) 0.101(6) Uiso 0.35(4) 1 d PDU A 2 H1S3 H 0.1007 0.7369 1.0000 0.121 Uiso 0.35(4) 1 calc PR A 2 H1S4 H 0.0346 0.6097 0.9252 0.121 Uiso 0.35(4) 1 calc PR A 2 C2S' C -0.025(13) 0.627(8) 1.044(5) 0.103(7) Uiso 0.35(4) 1 d PDU A 2 H2S4 H -0.1079 0.5516 1.0180 0.155 Uiso 0.35(4) 1 calc PR A 2 H2S5 H -0.0546 0.6830 1.0939 0.155 Uiso 0.35(4) 1 calc PR A 2 H2S6 H 0.0720 0.6158 1.0695 0.155 Uiso 0.35(4) 1 calc PR A 2 N31 N 0.370(2) 0.9117(16) 0.9310(13) 0.050(3) Uani 1 1 d U C . C32 C 0.369(3) 1.024(2) 0.9971(16) 0.049(3) Uiso 1 1 d U . . C36 C 0.507(3) 0.894(2) 0.9381(17) 0.053(3) Uiso 1 1 d U . . C37 C 0.194(3) 1.038(2) 0.9852(18) 0.062(5) Uiso 1 1 d U C . H37A H 0.1743 1.0750 1.0469 0.093 Uiso 1 1 calc R . . H37B H 0.1170 0.9603 0.9525 0.093 Uiso 1 1 calc R . . H37C H 0.1860 1.0863 0.9493 0.093 Uiso 1 1 calc R . . C40 C 0.518(3) 0.778(2) 0.8727(18) 0.062(5) Uiso 1 1 d U C . H40A H 0.4199 0.7161 0.8593 0.094 Uiso 1 1 calc R . . H40B H 0.6035 0.7583 0.9024 0.094 Uiso 1 1 calc R . . H40C H 0.5388 0.7840 0.8145 0.094 Uiso 1 1 calc R . . O1A O 0.535(3) 0.497(2) 0.3011(17) 0.098(4) Uani 1 1 d U B . O1B O 0.288(3) 0.453(2) 0.2297(16) 0.099(4) Uani 1 1 d U B . C1 C 0.441(5) 0.488(3) 0.238(2) 0.101(3) Uani 1 1 d DU . . C2 C 0.494(3) 0.5502(19) 0.1709(15) 0.104(3) Uiso 0.619(16) 1 d PDU B 1 C3 C 0.509(3) 0.684(2) 0.2148(17) 0.107(3) Uiso 0.619(16) 1 d PDU B 1 C4 C 0.575(3) 0.756(2) 0.1573(17) 0.111(4) Uiso 0.619(16) 1 d PDU B 1 F2A F 0.384(4) 0.517(3) 0.0903(19) 0.105(5) Uiso 0.619(16) 1 d PDU B 1 F2B F 0.646(3) 0.548(3) 0.170(2) 0.103(5) Uiso 0.619(16) 1 d PDU B 1 F4B F 0.728(3) 0.764(3) 0.154(3) 0.115(5) Uiso 0.619(16) 1 d PDU B 1 F4C F 0.573(5) 0.870(2) 0.194(2) 0.116(5) Uiso 0.619(16) 1 d PDU B 1 F3A F 0.361(3) 0.692(3) 0.216(2) 0.110(5) Uiso 0.619(16) 1 d PDU B 1 F3B F 0.596(5) 0.743(3) 0.3051(18) 0.110(4) Uiso 0.619(16) 1 d PDU B 1 F4A F 0.501(4) 0.701(3) 0.0644(18) 0.113(5) Uiso 0.619(16) 1 d PDU B 1 C2' C 0.488(4) 0.5571(17) 0.1743(16) 0.104(3) Uiso 0.381(16) 1 d PDU B 2 C3' C 0.541(4) 0.6933(16) 0.2023(15) 0.108(3) Uiso 0.381(16) 1 d PDU B 2 C4' C 0.588(3) 0.7847(19) 0.156(2) 0.112(4) Uiso 0.381(16) 1 d PDU B 2 F2Y F 0.598(6) 0.513(5) 0.134(4) 0.103(5) Uiso 0.381(16) 1 d PDU B 2 F3Y F 0.675(5) 0.726(5) 0.269(3) 0.109(5) Uiso 0.381(16) 1 d PDU B 2 F2Z F 0.422(7) 0.482(4) 0.083(2) 0.105(5) Uiso 0.381(16) 1 d PDU B 2 F3Z F 0.460(7) 0.735(5) 0.268(4) 0.109(5) Uiso 0.381(16) 1 d PDU B 2 F4Z F 0.437(4) 0.759(5) 0.110(4) 0.114(5) Uiso 0.381(16) 1 d PDU B 2 F4X F 0.699(6) 0.882(4) 0.224(3) 0.115(5) Uiso 0.381(16) 1 d PDU B 2 F4Y F 0.665(7) 0.724(5) 0.096(4) 0.113(5) Uiso 0.381(16) 1 d PDU B 2 O11A O -0.059(3) 0.8317(19) 0.7332(16) 0.097(3) Uiso 1 1 d U C 2 O11B O -0.324(3) 0.788(2) 0.6707(16) 0.095(4) Uani 1 1 d U . 2 C11 C -0.190(5) 0.8531(18) 0.713(3) 0.097(3) Uani 1 1 d DU C 2 C12 C -0.166(3) 0.9875(16) 0.7404(18) 0.113(3) Uiso 0.616(15) 1 d PDU D 1 C13 C -0.207(3) 1.063(2) 0.6855(18) 0.115(3) Uiso 0.616(15) 1 d PDU D 1 C14 C -0.120(3) 1.0307(19) 0.604(2) 0.117(4) Uiso 0.616(15) 1 d PDU D 1 F12B F -0.022(3) 1.049(3) 0.801(2) 0.113(4) Uiso 0.616(15) 1 d PDU D 1 F12A F -0.265(4) 1.016(3) 0.798(2) 0.110(4) Uiso 0.616(15) 1 d PDU D 1 F13B F -0.350(3) 1.010(3) 0.623(2) 0.120(5) Uiso 0.616(15) 1 d PDU D 1 F13A F -0.139(5) 1.182(2) 0.727(2) 0.116(5) Uiso 0.616(15) 1 d PDU D 1 F14A F -0.206(4) 0.917(2) 0.549(2) 0.116(5) Uiso 0.616(15) 1 d PDU D 1 F14B F -0.128(5) 1.123(3) 0.580(3) 0.121(5) Uiso 0.616(15) 1 d PDU D 1 F14C F 0.021(4) 1.034(3) 0.651(2) 0.118(4) Uiso 0.616(15) 1 d PDU D 1 C12' C -0.172(3) 0.9869(16) 0.742(2) 0.113(3) Uiso 0.384(15) 1 d PDU C 2 C13' C -0.064(4) 1.072(2) 0.7063(15) 0.115(3) Uiso 0.384(15) 1 d PDU C 2 C14' C -0.091(3) 1.0451(19) 0.5990(14) 0.117(4) Uiso 0.384(15) 1 d PDU C 2 F12Y F -0.077(6) 1.058(5) 0.828(3) 0.112(5) Uiso 0.384(15) 1 d PDU C 2 F13Y F -0.193(5) 0.996(3) 0.637(3) 0.117(4) Uiso 0.384(15) 1 d PDU C 2 F13Z F -0.072(7) 1.176(2) 0.701(4) 0.118(4) Uiso 0.384(15) 1 d PDU C 2 F12Z F -0.311(4) 1.005(5) 0.757(4) 0.109(5) Uiso 0.384(15) 1 d PDU C 2 F14Z F -0.076(6) 0.934(2) 0.572(3) 0.116(4) Uiso 0.384(15) 1 d PDU C 2 F14X F 0.039(4) 1.130(3) 0.661(3) 0.119(4) Uiso 0.384(15) 1 d PDU C 2 F14Y F -0.141(6) 1.072(4) 0.525(2) 0.116(5) Uiso 0.384(15) 1 d PDU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.092(2) 0.0707(16) 0.0790(17) 0.0341(13) 0.0291(14) 0.0314(13) Ag2 0.133(3) 0.0730(17) 0.0857(19) 0.0470(14) 0.0459(17) 0.0432(16) N21 0.081(7) 0.046(5) 0.075(6) 0.037(4) 0.032(5) 0.027(5) N24 0.080(7) 0.045(5) 0.074(6) 0.041(4) 0.030(5) 0.027(5) C23 0.081(7) 0.046(5) 0.074(6) 0.039(4) 0.031(5) 0.027(5) C22 0.081(7) 0.045(5) 0.075(6) 0.037(4) 0.031(5) 0.027(5) C26 0.080(7) 0.045(5) 0.074(6) 0.040(4) 0.031(5) 0.027(5) C25 0.080(7) 0.045(5) 0.074(6) 0.040(4) 0.030(5) 0.027(5) C27 0.085(9) 0.045(7) 0.079(8) 0.033(7) 0.029(8) 0.025(7) C30 0.083(9) 0.047(7) 0.079(8) 0.036(7) 0.029(8) 0.025(7) C28 0.085(9) 0.049(7) 0.075(8) 0.042(6) 0.030(8) 0.021(7) C29 0.082(9) 0.046(7) 0.080(8) 0.040(7) 0.034(8) 0.022(7) O1S 0.100(6) 0.100(6) 0.100(6) 0.041(3) 0.024(3) 0.031(3) N31 0.051(4) 0.050(4) 0.051(4) 0.021(3) 0.011(2) 0.017(3) O1A 0.101(5) 0.100(5) 0.101(5) 0.045(4) 0.027(4) 0.033(4) O1B 0.101(5) 0.100(5) 0.101(5) 0.045(4) 0.027(4) 0.030(4) C1 0.102(4) 0.101(4) 0.102(4) 0.043(3) 0.025(2) 0.032(3) O11B 0.106(5) 0.104(5) 0.106(5) 0.062(4) 0.041(4) 0.048(4) C11 0.107(4) 0.106(4) 0.107(4) 0.060(2) 0.040(2) 0.049(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N31 2.318(19) . ? Ag1 N21 2.32(2) . ? Ag1 O1S 2.36(2) . ? Ag1 O11A 2.44(3) . ? Ag2 N24 2.27(2) . ? Ag2 O11B 2.30(2) 2_566 ? Ag2 O1B 2.49(2) . ? Ag2 O1A 2.56(2) . ? N21 C26 1.30(3) . ? N21 C22 1.33(3) . ? N24 C25 1.34(3) . ? N24 C23 1.37(3) . ? C23 C22 1.41(4) . ? C23 C28 1.47(4) . ? C22 C27 1.51(3) . ? C26 C25 1.38(4) . ? C26 C29 1.57(3) . ? C25 C30 1.55(3) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O1S C1S 1.4101(12) . ? O1S C1S' 1.4105(12) . ? C1S C2S 1.5402(12) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C1S' C2S' 1.5400(16) . ? C1S' H1S3 0.9700 . ? C1S' H1S4 0.9700 . ? C2S' H2S4 0.9613 . ? C2S' H2S5 0.9614 . ? C2S' H2S6 0.9613 . ? N31 C36 1.28(3) . ? N31 C32 1.43(3) . ? C32 C36 1.32(3) 2_677 ? C32 C37 1.60(4) . ? C36 C32 1.32(3) 2_677 ? C36 C40 1.49(3) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? O1A C1 1.16(4) . ? O1B C1 1.30(4) . ? C1 C2' 1.5400(12) . ? C1 C2 1.5402(12) . ? C2 F2A 1.3503(12) . ? C2 F2B 1.3501(12) . ? C2 C3 1.5399(12) . ? C3 F3A 1.3500(12) . ? C3 F3B 1.3500(12) . ? C3 C4 1.5399(12) . ? C4 F4C 1.3500(12) . ? C4 F4A 1.3500(12) . ? C4 F4B 1.3500(12) . ? C2' F2Z 1.3500(12) . ? C2' F2Y 1.3501(12) . ? C2' C3' 1.5401(12) . ? C3' F3Y 1.3498(13) . ? C3' F3Z 1.3505(12) . ? C3' C4' 1.5402(12) . ? C4' F4X 1.3497(12) . ? C4' F4Z 1.3500(12) . ? C4' F4Y 1.3502(12) . ? O11A C11 1.28(4) . ? O11B C11 1.21(4) . ? O11B Ag2 2.30(2) 2_566 ? C11 C12' 1.5400(9) . ? C12 F12A 1.3502(12) . ? C12 F12B 1.3500(13) . ? C12 C13 1.5402(12) . ? C13 F13A 1.3500(13) . ? C13 F13B 1.3498(13) . ? C13 C14 1.5400(12) . ? C14 F14C 1.3502(12) . ? C14 F14A 1.3501(12) . ? C14 F14B 1.3500(12) . ? C12' F12Y 1.3500(13) . ? C12' F12Z 1.3501(12) . ? C12' C13' 1.5400(12) . ? C13' F13Y 1.3502(13) . ? C13' F13Z 1.3501(12) . ? C13' C14' 1.5400(12) . ? C14' F14X 1.3500(13) . ? C14' F14Z 1.3500(12) . ? C14' F14Y 1.3501(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Ag1 N21 120.6(8) . . ? N31 Ag1 O1S 104.4(7) . . ? N21 Ag1 O1S 124.8(7) . . ? N31 Ag1 O11A 126.2(7) . . ? N21 Ag1 O11A 91.2(8) . . ? O1S Ag1 O11A 85.9(8) . . ? N24 Ag2 O11B 129.1(7) . 2_566 ? N24 Ag2 O1B 118.6(7) . . ? O11B Ag2 O1B 108.3(8) 2_566 . ? N24 Ag2 O1A 121.4(7) . . ? O11B Ag2 O1A 102.7(8) 2_566 . ? O1B Ag2 O1A 51.1(8) . . ? C26 N21 C22 120(2) . . ? C26 N21 Ag1 121.6(16) . . ? C22 N21 Ag1 117.6(15) . . ? C25 N24 C23 118(2) . . ? C25 N24 Ag2 121.7(15) . . ? C23 N24 Ag2 120.7(16) . . ? N24 C23 C22 118(2) . . ? N24 C23 C28 119(2) . . ? C22 C23 C28 122(2) . . ? N21 C22 C23 121(2) . . ? N21 C22 C27 119(2) . . ? C23 C22 C27 119(2) . . ? N21 C26 C25 120(2) . . ? N21 C26 C29 119(2) . . ? C25 C26 C29 120.5(19) . . ? N24 C25 C26 122(2) . . ? N24 C25 C30 115(2) . . ? C26 C25 C30 122(2) . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C30 H30A 109.4 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.4 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.4 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C1S O1S C1S' 21(4) . . ? C1S O1S Ag1 131(2) . . ? C1S' O1S Ag1 121(2) . . ? O1S C1S C2S 107(3) . . ? O1S C1S H1S1 110.3 . . ? C2S C1S H1S1 110.3 . . ? O1S C1S H1S2 110.4 . . ? C2S C1S H1S2 110.4 . . ? H1S1 C1S H1S2 108.5 . . ? O1S C1S' C2S' 156.7(4) . . ? O1S C1S' H1S3 97.0 . . ? C2S' C1S' H1S3 97.0 . . ? O1S C1S' H1S4 97.0 . . ? C2S' C1S' H1S4 97.7 . . ? H1S3 C1S' H1S4 103.5 . . ? C1S' C2S' H2S4 109.4 . . ? C1S' C2S' H2S5 110.2 . . ? H2S4 C2S' H2S5 109.3 . . ? C1S' C2S' H2S6 109.2 . . ? H2S4 C2S' H2S6 109.3 . . ? H2S5 C2S' H2S6 109.4 . . ? C36 N31 C32 114(2) . . ? C36 N31 Ag1 122.7(16) . . ? C32 N31 Ag1 122.6(16) . . ? C36 C32 N31 125(2) 2_677 . ? C36 C32 C37 124(2) 2_677 . ? N31 C32 C37 111(2) . . ? N31 C36 C32 121(2) . 2_677 ? N31 C36 C40 118(2) . . ? C32 C36 C40 122(2) 2_677 . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.4 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C1 O1A Ag2 92.2(19) . . ? C1 O1B Ag2 92.0(16) . . ? O1A C1 O1B 124(2) . . ? O1A C1 C2' 120(3) . . ? O1B C1 C2' 112(3) . . ? O1A C1 C2 119(3) . . ? O1B C1 C2 115(3) . . ? F2A C2 F2B 122(3) . . ? F2A C2 C3 99(2) . . ? F2B C2 C3 104(2) . . ? F2A C2 C1 114(3) . . ? F2B C2 C1 105(3) . . ? C3 C2 C1 111(2) . . ? F3A C3 F3B 107(3) . . ? F3A C3 C4 105(2) . . ? F3B C3 C4 107(2) . . ? F3A C3 C2 107(2) . . ? F3B C3 C2 115(2) . . ? C4 C3 C2 114.8(19) . . ? F4C C4 F4A 112(3) . . ? F4C C4 F4B 106(3) . . ? F4A C4 F4B 102(3) . . ? F4C C4 C3 112(2) . . ? F4A C4 C3 111(2) . . ? F4B C4 C3 113(3) . . ? F2Z C2' F2Y 70(4) . . ? F2Z C2' C1 108(3) . . ? F2Y C2' C1 105(3) . . ? F2Z C2' C3' 120(3) . . ? F2Y C2' C3' 109(3) . . ? C1 C2' C3' 128(2) . . ? F3Y C3' F3Z 92(4) . . ? F3Y C3' C4' 101(3) . . ? F3Z C3' C4' 108(3) . . ? F3Y C3' C2' 100(3) . . ? F3Z C3' C2' 105(3) . . ? C4' C3' C2' 139.5(2) . . ? F4X C4' F4Z 136(4) . . ? F4X C4' F4Y 108(4) . . ? F4Z C4' F4Y 109(4) . . ? F4X C4' C3' 106(3) . . ? F4Z C4' C3' 93(3) . . ? F4Y C4' C3' 96(3) . . ? C11 O11A Ag1 161(2) . . ? C11 O11B Ag2 107.9(17) . 2_566 ? O11B C11 O11A 132(2) . . ? O11B C11 C12' 114(3) . . ? O11A C11 C12' 114(3) . . ? F12A C12 F12B 101(3) . . ? F12A C12 C13 92(2) . . ? F12B C12 C13 108(2) . . ? F13A C13 F13B 124(3) . . ? F13A C13 C14 101(2) . . ? F13B C13 C14 91(2) . . ? F13A C13 C12 117(2) . . ? F13B C13 C12 113(2) . . ? C14 C13 C12 102(2) . . ? F14C C14 F14A 110(3) . . ? F14C C14 F14B 119(3) . . ? F14A C14 F14B 122(3) . . ? F14C C14 C13 101(3) . . ? F14A C14 C13 103(2) . . ? F14B C14 C13 95(2) . . ? F12Y C12' F12Z 100(4) . . ? F12Y C12' C11 114(4) . . ? F12Z C12' C11 109(3) . . ? F12Y C12' C13' 85(3) . . ? F12Z C12' C13' 118(3) . . ? C11 C12' C13' 126(3) . . ? F13Y C13' F13Z 99.43(11) . . ? F13Y C13' C12' 69(3) . . ? F13Z C13' C12' 131(4) . . ? F13Y C13' C14' 52(3) . . ? F13Z C13' C14' 76(3) . . ? C12' C13' C14' 119(2) . . ? F14X C14' F14Z 112.89(14) . . ? F14X C14' F14Y 112.89(14) . . ? F14Z C14' F14Y 112.87(14) . . ? F14X C14' C13' 59(2) . . ? F14Z C14' C13' 96(2) . . ? F14Y C14' C13' 150(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.316 _refine_diff_density_min -1.891 _refine_diff_density_rms 0.389