# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Boomishankar Ramamoorthy' _publ_contact_author_email 'boomi@iiserpune.ac.in, boomi.iiser@gmail.com' loop_ _publ_author_name 'Arvind Gupta' 'Alexander Steiner' 'Boomishankar Ramamoorthy' # Attachment '- compound1_new.cif' data_trial-a _database_code_depnum_ccdc_archive 'CCDC 865262' #TrackingRef '- compound1_new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H15 N6 O P, C7H8' _chemical_formula_sum 'C22 H23 N6 O P' _chemical_formula_weight 418.43 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' 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.975(3) _cell_length_b 17.625(2) _cell_length_c 29.216(3) _cell_angle_alpha 90.00 _cell_angle_beta 130.373(6) _cell_angle_gamma 90.00 _cell_volume 8620.7(18) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 28.41 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 Apex II' _diffrn_measurement_method 'Omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 122944 _diffrn_reflns_av_R_equivalents 0.1152 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 4.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 15154 _reflns_number_gt 9343 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Four carbon atoms of one of the pyridyl rings One of the toluene molecules in 1.C7H8 was disordered.It was split over two positions and refined isotropically with occupancy factors and similar-distance and similar U restraints.Two carbon atoms (C36 and C46) had slightlty bad ADPs and therefore refined with partial isotropic factors. ; _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^)+(0.0527P)^2^+9.3248P] 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 15154 _refine_ls_number_parameters 1039 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1414 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.005 _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 P1 P 0.41541(5) 0.05526(4) 0.22832(3) 0.01629(18) Uani 1 1 d . . . P2 P 0.44999(5) 0.36074(4) 0.26973(3) 0.01530(18) Uani 1 1 d . . . P3 P 0.07802(5) 0.70275(4) 0.26478(3) 0.01624(18) Uani 1 1 d . . . P4 P 0.04540(5) 0.39675(4) 0.22461(4) 0.01812(19) Uani 1 1 d . . . O1 O 0.41848(12) -0.02327(11) 0.24733(9) 0.0197(5) Uani 1 1 d . . . O2 O 0.42257(12) 0.43985(11) 0.25109(9) 0.0181(5) Uani 1 1 d . . . O3 O 0.07441(12) 0.78134(11) 0.24590(9) 0.0190(5) Uani 1 1 d . . . O4 O 0.07443(12) 0.31802(11) 0.24360(10) 0.0216(5) Uani 1 1 d . . . N1 N 0.33015(14) 0.08067(14) 0.16298(11) 0.0167(6) Uani 1 1 d . . . H1 H 0.3074 0.1217 0.1630 0.020 Uiso 1 1 calc R . . N2 N 0.42707(15) 0.12119(14) 0.27379(11) 0.0184(6) Uani 1 1 d . . . H2 H 0.4682 0.1519 0.2910 0.022 Uiso 1 1 calc R . . N3 N 0.48934(14) 0.06963(14) 0.22806(11) 0.0184(6) Uani 1 1 d . . . H3 H 0.5282 0.0360 0.2481 0.022 Uiso 1 1 calc R . . N4 N 0.53264(14) 0.34799(14) 0.28048(11) 0.0170(6) Uani 1 1 d . . . H4 H 0.5422 0.3817 0.2636 0.020 Uiso 1 1 calc R . . N5 N 0.38687(14) 0.29594(14) 0.21983(10) 0.0162(6) Uani 1 1 d . . . H5 H 0.4059 0.2625 0.2096 0.019 Uiso 1 1 calc R . . N6 N 0.46300(14) 0.33684(14) 0.32994(10) 0.0170(6) Uani 1 1 d . . . H6 H 0.4450 0.2920 0.3295 0.020 Uiso 1 1 calc R . . N7 N 0.16382(14) 0.67660(14) 0.32880(11) 0.0182(6) Uani 1 1 d . . . H7 H 0.1865 0.6361 0.3280 0.022 Uiso 1 1 calc R . . N8 N 0.00591(14) 0.68855(14) 0.26706(11) 0.0172(6) Uani 1 1 d . . . H8 H -0.0335 0.7215 0.2471 0.021 Uiso 1 1 calc R . . N9 N 0.06468(15) 0.63740(14) 0.21833(11) 0.0194(6) Uani 1 1 d . . . H9 H 0.0236 0.6068 0.2017 0.023 Uiso 1 1 calc R . . N10 N 0.03037(15) 0.42119(15) 0.16382(11) 0.0215(6) Uani 1 1 d . . . H10 H 0.0470 0.4668 0.1643 0.026 Uiso 1 1 calc R . . N11 N 0.10868(14) 0.46196(14) 0.27409(11) 0.0182(6) Uani 1 1 d . . . H11 H 0.0904 0.4950 0.2852 0.022 Uiso 1 1 calc R . . N12 N -0.03536(14) 0.40831(14) 0.21625(11) 0.0194(6) Uani 1 1 d . . . H12 H -0.0436 0.3737 0.2335 0.023 Uiso 1 1 calc R . . C11 C 0.29026(17) 0.04479(17) 0.10801(13) 0.0173(7) Uani 1 1 d . . . N12P N 0.30785(15) -0.02777(15) 0.10814(11) 0.0217(6) Uani 1 1 d . . . C46 C 0.66594(18) 0.30273(18) 0.33329(14) 0.0215(7) Uani 1 1 d U . . H46 H 0.6791 0.3485 0.3243 0.026 Uiso 1 1 calc R . . C13 C 0.2670(2) -0.0624(2) 0.05471(14) 0.0267(8) Uani 1 1 d . . . H13 H 0.2793 -0.1139 0.0542 0.032 Uiso 1 1 calc R . . C14 C 0.2087(2) -0.0281(2) 0.00098(15) 0.0309(8) Uani 1 1 d . . . H14 H 0.1806 -0.0554 -0.0357 0.037 Uiso 1 1 calc R . . C15 C 0.1915(2) 0.0476(2) 0.00117(15) 0.0348(9) Uani 1 1 d . . . H15 H 0.1517 0.0733 -0.0354 0.042 Uiso 1 1 calc R . . C16 C 0.2328(2) 0.08466(19) 0.05523(15) 0.0273(8) Uani 1 1 d . . . H16 H 0.2224 0.1366 0.0566 0.033 Uiso 1 1 calc R . . C21 C 0.37734(18) 0.13238(17) 0.28729(13) 0.0184(7) Uani 1 1 d . . . N22P N 0.39206(16) 0.19483(15) 0.31876(11) 0.0217(6) Uani 1 1 d . . . C23 C 0.3437(2) 0.20966(19) 0.33095(15) 0.0270(8) Uani 1 1 d . . . H23 H 0.3542 0.2538 0.3537 0.032 Uiso 1 1 calc R . . C24 C 0.2804(2) 0.1650(2) 0.31257(16) 0.0311(8) Uani 1 1 d . . . H24 H 0.2464 0.1788 0.3207 0.037 Uiso 1 1 calc R . . C25 C 0.2677(2) 0.0989(2) 0.28165(15) 0.0281(8) Uani 1 1 d . . . H25 H 0.2254 0.0657 0.2692 0.034 Uiso 1 1 calc R . . C26 C 0.31651(18) 0.08177(18) 0.26916(14) 0.0224(7) Uani 1 1 d . . . H26 H 0.3090 0.0363 0.2486 0.027 Uiso 1 1 calc R . . C31 C 0.49921(18) 0.12742(17) 0.20066(13) 0.0174(7) Uani 1 1 d . . . N32P N 0.45506(14) 0.19012(14) 0.18391(11) 0.0177(6) Uani 1 1 d . . . C33 C 0.46400(19) 0.24447(18) 0.15627(14) 0.0219(7) Uani 1 1 d . . . H33 H 0.4327 0.2892 0.1439 0.026 Uiso 1 1 calc R . . C34 C 0.5154(2) 0.23939(19) 0.14490(15) 0.0279(8) Uani 1 1 d . . . H34 H 0.5192 0.2790 0.1248 0.033 Uiso 1 1 calc R . . C35 C 0.5620(2) 0.1741(2) 0.16382(16) 0.0298(8) Uani 1 1 d . . . H35 H 0.5989 0.1687 0.1574 0.036 Uiso 1 1 calc R . . C36 C 0.55367(19) 0.11761(19) 0.19198(14) 0.0238(7) Uani 1 1 d U . . H36 H 0.5848 0.0726 0.2052 0.029 Uiso 1 1 calc R . . C41 C 0.58943(17) 0.29081(17) 0.31287(13) 0.0165(7) Uani 1 1 d . . . N42P N 0.56681(15) 0.22624(14) 0.32284(11) 0.0169(6) Uani 1 1 d . . . C43 C 0.62374(18) 0.17254(18) 0.35561(13) 0.0199(7) Uani 1 1 d . . . H43 H 0.6092 0.1265 0.3632 0.024 Uiso 1 1 calc R . . C44 C 0.70096(19) 0.18008(19) 0.37854(14) 0.0236(8) Uani 1 1 d . . . H44 H 0.7389 0.1408 0.4018 0.028 Uiso 1 1 calc R . . C45 C 0.72216(19) 0.24696(19) 0.36674(15) 0.0256(8) Uani 1 1 d . . . H45 H 0.7751 0.2540 0.3817 0.031 Uiso 1 1 calc R . . C51 C 0.30649(17) 0.28899(17) 0.19233(13) 0.0158(6) Uani 1 1 d . . . N52P N 0.27110(15) 0.22578(14) 0.16122(11) 0.0200(6) Uani 1 1 d . . . C53 C 0.19409(18) 0.21566(19) 0.13494(15) 0.0255(8) Uani 1 1 d . . . H53 H 0.1687 0.1703 0.1128 0.031 Uiso 1 1 calc R . . C54 C 0.14960(19) 0.26686(19) 0.13803(15) 0.0281(8) Uani 1 1 d . . . H54 H 0.0953 0.2571 0.1191 0.034 Uiso 1 1 calc R . . C55 C 0.18731(19) 0.33337(19) 0.16998(15) 0.0263(8) Uani 1 1 d . . . H55 H 0.1587 0.3705 0.1729 0.032 Uiso 1 1 calc R . . C56 C 0.26584(19) 0.34541(19) 0.19720(14) 0.0227(7) Uani 1 1 d . . . H56 H 0.2922 0.3909 0.2189 0.027 Uiso 1 1 calc R . . C61 C 0.49978(18) 0.38046(17) 0.38196(13) 0.0183(7) Uani 1 1 d . . . N62P N 0.48997(15) 0.35455(15) 0.41977(11) 0.0230(6) Uani 1 1 d . . . C63 C 0.52251(19) 0.3959(2) 0.46932(15) 0.0271(8) Uani 1 1 d . . . H63 H 0.5156 0.3786 0.4965 0.032 Uiso 1 1 calc R . . C64 C 0.5650(2) 0.4614(2) 0.48344(15) 0.0289(8) Uani 1 1 d . . . H64 H 0.5864 0.4887 0.5191 0.035 Uiso 1 1 calc R . . C65 C 0.57586(19) 0.48650(19) 0.44440(14) 0.0263(8) Uani 1 1 d . . . H65 H 0.6056 0.5314 0.4531 0.032 Uiso 1 1 calc R . . C66 C 0.54349(18) 0.44629(18) 0.39285(14) 0.0214(7) Uani 1 1 d . . . H66 H 0.5504 0.4625 0.3655 0.026 Uiso 1 1 calc R . . C71 C 0.20437(17) 0.71231(17) 0.38444(13) 0.0179(7) Uani 1 1 d . . . N72P N 0.17995(15) 0.78186(15) 0.38377(11) 0.0214(6) Uani 1 1 d . . . C73 C 0.2213(2) 0.8175(2) 0.43686(14) 0.0266(8) Uani 1 1 d . . . H73 H 0.2052 0.8673 0.4373 0.032 Uiso 1 1 calc R . . C74 C 0.2854(2) 0.7866(2) 0.49046(15) 0.0315(9) Uani 1 1 d . . . H74 H 0.3137 0.8147 0.5268 0.038 Uiso 1 1 calc R . . C75 C 0.3077(2) 0.7128(2) 0.49025(15) 0.0301(8) Uani 1 1 d . . . H75 H 0.3509 0.6889 0.5267 0.036 Uiso 1 1 calc R . . C76 C 0.26640(19) 0.67519(19) 0.43653(14) 0.0248(8) Uani 1 1 d . . . H76 H 0.2801 0.6246 0.4351 0.030 Uiso 1 1 calc R . . C81 C -0.00086(17) 0.63103(17) 0.29646(13) 0.0170(7) Uani 1 1 d . . . N82P N 0.04189(15) 0.56788(14) 0.31131(11) 0.0197(6) Uani 1 1 d . . . C83 C 0.03477(18) 0.51361(18) 0.34045(13) 0.0203(7) Uani 1 1 d . . . H83 H 0.0654 0.4686 0.3519 0.024 Uiso 1 1 calc R . . C84 C -0.01353(19) 0.51942(19) 0.35439(14) 0.0252(8) Uani 1 1 d . . . H84 H -0.0163 0.4798 0.3751 0.030 Uiso 1 1 calc R . . C85 C -0.05852(19) 0.58513(19) 0.33733(15) 0.0247(8) Uani 1 1 d . . . H85 H -0.0935 0.5908 0.3457 0.030 Uiso 1 1 calc R . . C86 C -0.05231(19) 0.64220(18) 0.30822(14) 0.0221(7) Uani 1 1 d . . . H86 H -0.0822 0.6877 0.2966 0.027 Uiso 1 1 calc R . . C91 C 0.11239(18) 0.62637(18) 0.20313(14) 0.0199(7) Uani 1 1 d . . . N92P N 0.09507(17) 0.56557(15) 0.16950(12) 0.0260(6) Uani 1 1 d . . . C93 C 0.1406(2) 0.5516(2) 0.15496(17) 0.0368(9) Uani 1 1 d . . . H93 H 0.1280 0.5086 0.1306 0.044 Uiso 1 1 calc R . . C94 C 0.2043(2) 0.5955(2) 0.17306(18) 0.0376(9) Uani 1 1 d . . . H94 H 0.2358 0.5827 0.1624 0.045 Uiso 1 1 calc R . . C95 C 0.2213(2) 0.6589(2) 0.20731(16) 0.0319(8) Uani 1 1 d . . . H95 H 0.2644 0.6912 0.2202 0.038 Uiso 1 1 calc R . . C96 C 0.17534(19) 0.67526(19) 0.22267(14) 0.0249(8) Uani 1 1 d . . . H96 H 0.1861 0.7188 0.2461 0.030 Uiso 1 1 calc R . . C101 C -0.00538(18) 0.37909(19) 0.11134(15) 0.0249(8) Uani 1 1 d . . . N102 N 0.00265(17) 0.40995(17) 0.07355(12) 0.0301(7) Uani 1 1 d . . . C103 C -0.0296(2) 0.3721(2) 0.02269(16) 0.0394(10) Uani 1 1 d . . . H103 H -0.0241 0.3932 -0.0044 0.047 Uiso 1 1 calc R . . C104 C -0.0705(2) 0.3041(3) 0.00712(17) 0.0442(11) Uani 1 1 d . . . H104 H -0.0921 0.2790 -0.0294 0.053 Uiso 1 1 calc R . . C105 C -0.0787(2) 0.2741(2) 0.04664(18) 0.0406(10) Uani 1 1 d . . . H105 H -0.1069 0.2279 0.0372 0.049 Uiso 1 1 calc R . . C106 C -0.04588(19) 0.3113(2) 0.09971(16) 0.0299(8) Uani 1 1 d . . . H106 H -0.0508 0.2914 0.1274 0.036 Uiso 1 1 calc R . . C111 C 0.18846(18) 0.46923(17) 0.29968(13) 0.0170(7) Uani 1 1 d . . . N112 N 0.22303(14) 0.53469(14) 0.32776(11) 0.0186(6) Uani 1 1 d . . . C113 C 0.29891(18) 0.54582(18) 0.35188(14) 0.0207(7) Uani 1 1 d . . . H113 H 0.3233 0.5928 0.3715 0.025 Uiso 1 1 calc R . . C114 C 0.34337(18) 0.49364(18) 0.34999(14) 0.0209(7) Uani 1 1 d . . . H114 H 0.3968 0.5042 0.3672 0.025 Uiso 1 1 calc R . . C115 C 0.30751(19) 0.42485(19) 0.32208(14) 0.0231(7) Uani 1 1 d . . . H115 H 0.3366 0.3869 0.3203 0.028 Uiso 1 1 calc R . . C116 C 0.22956(18) 0.41183(18) 0.29695(14) 0.0221(7) Uani 1 1 d . . . H116 H 0.2044 0.3647 0.2782 0.027 Uiso 1 1 calc R . . C121 C -0.09283(18) 0.46545(17) 0.18559(13) 0.0178(7) Uani 1 1 d . . . N122 N -0.07311(15) 0.52970(14) 0.17359(11) 0.0198(6) Uani 1 1 d . . . C123 C -0.13049(19) 0.58337(19) 0.14254(14) 0.0245(8) Uani 1 1 d . . . H123 H -0.1178 0.6292 0.1332 0.029 Uiso 1 1 calc R . . C124 C -0.2053(2) 0.57609(19) 0.12381(15) 0.0271(8) Uani 1 1 d . . . H124 H -0.2436 0.6154 0.1018 0.033 Uiso 1 1 calc R . . C125 C -0.22416(19) 0.5093(2) 0.13786(15) 0.0278(8) Uani 1 1 d . . . H125 H -0.2756 0.5025 0.1259 0.033 Uiso 1 1 calc R . . C126 C -0.16762(18) 0.45362(18) 0.16908(14) 0.0223(7) Uani 1 1 d . . . H126 H -0.1790 0.4078 0.1793 0.027 Uiso 1 1 calc R . . C1S C 0.2693(3) 0.2872(3) 0.45075(19) 0.0497(11) Uani 1 1 d . . . C2S C 0.1935(3) 0.3081(2) 0.40003(18) 0.0471(11) Uani 1 1 d . . . H2S H 0.1871 0.3368 0.3696 0.056 Uiso 1 1 calc R . . C3S C 0.1271(3) 0.2881(2) 0.39264(18) 0.0455(11) Uani 1 1 d . . . H3S H 0.0755 0.3026 0.3572 0.055 Uiso 1 1 calc R . . C4S C 0.1355(3) 0.2470(2) 0.4367(2) 0.0479(11) Uani 1 1 d . . . H4S H 0.0899 0.2339 0.4321 0.058 Uiso 1 1 calc R . . C5S C 0.2107(3) 0.2253(2) 0.48745(19) 0.0492(11) Uani 1 1 d . . . H5S H 0.2170 0.1965 0.5178 0.059 Uiso 1 1 calc R . . C6S C 0.2765(3) 0.2453(3) 0.49418(18) 0.0509(12) Uani 1 1 d . . . H6S H 0.3280 0.2300 0.5293 0.061 Uiso 1 1 calc R . . C7S C 0.3416(3) 0.3091(4) 0.4585(2) 0.0861(19) Uani 1 1 d . . . H7S1 H 0.3898 0.2898 0.4971 0.129 Uiso 1 1 calc R . . H7S2 H 0.3447 0.3645 0.4577 0.129 Uiso 1 1 calc R . . H7S3 H 0.3376 0.2872 0.4258 0.129 Uiso 1 1 calc R . . C8S C 0.0574(2) 0.8898(2) 0.04891(17) 0.0370(9) Uani 1 1 d . . . C9S C 0.0291(2) 0.8442(2) 0.07071(19) 0.0384(10) Uani 1 1 d . . . H9S H -0.0213 0.8200 0.0430 0.046 Uiso 1 1 calc R . . C10S C 0.0717(3) 0.8337(2) 0.13003(19) 0.0453(10) Uani 1 1 d . . . H10S H 0.0510 0.8020 0.1434 0.054 Uiso 1 1 calc R . . C11S C 0.1462(3) 0.8690(2) 0.1725(2) 0.0497(11) Uani 1 1 d . . . H11S H 0.1759 0.8625 0.2144 0.060 Uiso 1 1 calc R . . C12S C 0.1742(2) 0.9128(2) 0.1514(2) 0.0504(12) Uani 1 1 d . . . H12S H 0.2246 0.9369 0.1792 0.060 Uiso 1 1 calc R . . C13S C 0.1318(2) 0.9232(2) 0.09083(18) 0.0349(9) Uani 1 1 d . . . H13S H 0.1537 0.9534 0.0776 0.042 Uiso 1 1 calc R . . C14S C 0.0093(3) 0.9013(3) -0.01644(18) 0.0540(12) Uani 1 1 d . . . H14A H -0.0412 0.8735 -0.0383 0.081 Uiso 1 1 calc R . . H14B H 0.0389 0.8825 -0.0286 0.081 Uiso 1 1 calc R . . H14C H -0.0018 0.9555 -0.0258 0.081 Uiso 1 1 calc R . . C15A C 0.22929(17) 0.46577(19) 0.04632(13) 0.0376(17) Uiso 0.628(5) 1 d PGDU A 1 C16A C 0.3009(2) 0.4512(2) 0.10361(12) 0.0406(19) Uiso 0.628(5) 1 d PGDU A 1 H16A H 0.3006 0.4316 0.1337 0.049 Uiso 0.628(5) 1 calc PR A 1 C17A C 0.37309(17) 0.4654(2) 0.11683(14) 0.0386(16) Uiso 0.628(5) 1 d PGDU A 1 H17A H 0.4221 0.4554 0.1560 0.046 Uiso 0.628(5) 1 calc PR A 1 C18A C 0.37360(18) 0.4940(2) 0.07275(17) 0.0457(18) Uiso 0.628(5) 1 d PGDU A 1 H18A H 0.4229 0.5037 0.0818 0.055 Uiso 0.628(5) 1 calc PR A 1 C19A C 0.3020(2) 0.5086(2) 0.01546(15) 0.0492(19) Uiso 0.628(5) 1 d PGDU A 1 H19A H 0.3023 0.5282 -0.0147 0.059 Uiso 0.628(5) 1 calc PR A 1 C20A C 0.22979(19) 0.4944(2) 0.00224(12) 0.0330(15) Uiso 0.628(5) 1 d PGDU A 1 H20A H 0.1808 0.5044 -0.0369 0.040 Uiso 0.628(5) 1 calc PR A 1 C21A C 0.1512(2) 0.4496(3) 0.0320(2) 0.057(2) Uiso 0.628(5) 1 d PGDU A 1 H21A H 0.1069 0.4629 -0.0099 0.086 Uiso 0.628(5) 1 calc PR A 1 H21B H 0.1478 0.4799 0.0585 0.086 Uiso 0.628(5) 1 calc PR A 1 H21C H 0.1483 0.3956 0.0383 0.086 Uiso 0.628(5) 1 calc PR A 1 C15B C 0.3090(2) 0.4715(2) 0.07115(17) 0.043(3) Uiso 0.372(5) 1 d PGDU A 2 C16B C 0.2556(2) 0.4945(3) 0.0114(2) 0.033(3) Uiso 0.372(5) 1 d PGDU A 2 H16B H 0.2748 0.5092 -0.0085 0.040 Uiso 0.372(5) 1 calc PR A 2 C17B C 0.1741(2) 0.4960(4) -0.0191(2) 0.046(3) Uiso 0.372(5) 1 d PGDU A 2 H17B H 0.1377 0.5117 -0.0599 0.055 Uiso 0.372(5) 1 calc PR A 2 C18B C 0.1460(2) 0.4745(4) 0.0100(2) 0.059(4) Uiso 0.372(5) 1 d PGDU A 2 H18B H 0.0903 0.4755 -0.0109 0.071 Uiso 0.372(5) 1 calc PR A 2 C19B C 0.1994(3) 0.4515(3) 0.0697(3) 0.050(3) Uiso 0.372(5) 1 d PGDU A 2 H19B H 0.1801 0.4369 0.0896 0.060 Uiso 0.372(5) 1 calc PR A 2 C20B C 0.2808(3) 0.4500(4) 0.1003(2) 0.034(3) Uiso 0.372(5) 1 d PGDU A 2 H20B H 0.3173 0.4343 0.1411 0.041 Uiso 0.372(5) 1 calc PR A 2 C21B C 0.3959(2) 0.4695(3) 0.10219(16) 0.059(4) Uiso 0.372(5) 1 d PGDU A 2 H21D H 0.4260 0.4524 0.1437 0.089 Uiso 0.372(5) 1 calc PR A 2 H21E H 0.4137 0.5204 0.1021 0.089 Uiso 0.372(5) 1 calc PR A 2 H21F H 0.4049 0.4344 0.0811 0.089 Uiso 0.372(5) 1 calc PR A 2 C22S C 0.5561(2) 0.3651(2) 0.04168(18) 0.0628(13) Uani 1 1 d G . . C23S C 0.53532(18) 0.41810(19) 0.06569(16) 0.0639(14) Uani 1 1 d G . . H23S H 0.4885 0.4477 0.0387 0.077 Uiso 1 1 calc R . . C24S C 0.5780(3) 0.4286(3) 0.1241(2) 0.0660(14) Uani 1 1 d . . . H24S H 0.5614 0.4643 0.1384 0.079 Uiso 1 1 calc R . . C25S C 0.6466(3) 0.3870(3) 0.1635(2) 0.0612(13) Uani 1 1 d . . . H25S H 0.6784 0.3952 0.2055 0.073 Uiso 1 1 calc R . . C26S C 0.6695(3) 0.3346(3) 0.1435(2) 0.0536(12) Uani 1 1 d . . . H26S H 0.7169 0.3060 0.1713 0.064 Uiso 1 1 calc R . . C27S C 0.6237(3) 0.3227(3) 0.0821(2) 0.0545(12) Uani 1 1 d . . . H27S H 0.6391 0.2852 0.0680 0.065 Uiso 1 1 calc R . . C28S C 0.5093(4) 0.3550(4) -0.0236(2) 0.095(2) Uani 1 1 d . . . H28A H 0.4632 0.3893 -0.0457 0.143 Uiso 1 1 calc R . . H28B H 0.4907 0.3024 -0.0347 0.143 Uiso 1 1 calc R . . H28C H 0.5430 0.3667 -0.0337 0.143 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 P1 0.0170(4) 0.0118(4) 0.0204(4) -0.0008(3) 0.0123(4) 0.0001(3) P2 0.0146(4) 0.0120(4) 0.0186(4) -0.0013(3) 0.0104(4) -0.0007(3) P3 0.0175(4) 0.0113(4) 0.0207(4) -0.0009(3) 0.0127(4) -0.0003(3) P4 0.0167(4) 0.0109(4) 0.0270(5) -0.0024(3) 0.0143(4) -0.0013(3) O1 0.0225(12) 0.0115(11) 0.0237(12) -0.0004(9) 0.0144(10) -0.0005(9) O2 0.0177(11) 0.0118(11) 0.0226(11) 0.0000(9) 0.0120(10) 0.0003(9) O3 0.0231(12) 0.0141(11) 0.0229(12) 0.0007(9) 0.0163(10) 0.0012(9) O4 0.0211(12) 0.0106(11) 0.0329(13) -0.0016(9) 0.0175(11) -0.0003(9) N1 0.0153(13) 0.0112(14) 0.0216(14) -0.0019(10) 0.0110(12) 0.0028(10) N2 0.0187(13) 0.0157(14) 0.0229(14) -0.0025(11) 0.0144(12) -0.0034(11) N3 0.0172(13) 0.0148(14) 0.0220(14) 0.0041(11) 0.0123(12) 0.0037(11) N4 0.0173(13) 0.0136(14) 0.0196(14) 0.0031(11) 0.0118(12) 0.0002(11) N5 0.0147(13) 0.0116(14) 0.0194(14) -0.0038(10) 0.0097(12) -0.0015(10) N6 0.0189(14) 0.0131(14) 0.0199(14) -0.0033(11) 0.0129(12) -0.0038(11) N7 0.0183(14) 0.0131(14) 0.0218(14) -0.0009(11) 0.0124(12) 0.0024(11) N8 0.0149(13) 0.0133(14) 0.0214(14) 0.0034(11) 0.0109(12) 0.0046(11) N9 0.0188(14) 0.0148(14) 0.0251(15) -0.0050(11) 0.0145(13) -0.0037(11) N10 0.0232(14) 0.0125(14) 0.0308(16) -0.0056(11) 0.0185(13) -0.0039(11) N11 0.0179(13) 0.0135(14) 0.0283(15) -0.0021(11) 0.0173(12) 0.0009(11) N12 0.0205(14) 0.0115(14) 0.0295(15) 0.0029(11) 0.0176(13) 0.0009(11) C11 0.0180(16) 0.0166(18) 0.0196(16) -0.0014(13) 0.0133(14) -0.0009(13) N12P 0.0216(14) 0.0186(15) 0.0239(15) -0.0035(12) 0.0142(13) 0.0013(12) C46 0.0205(10) 0.0207(11) 0.0226(10) -0.0008(8) 0.0137(8) -0.0012(8) C13 0.0308(19) 0.0216(19) 0.0281(19) -0.0056(15) 0.0192(17) -0.0004(15) C14 0.035(2) 0.029(2) 0.0219(19) -0.0061(15) 0.0154(17) 0.0004(17) C15 0.037(2) 0.034(2) 0.0200(19) 0.0042(16) 0.0127(17) 0.0082(17) C16 0.0325(19) 0.0184(19) 0.0280(19) 0.0017(14) 0.0182(17) 0.0028(15) C21 0.0220(17) 0.0145(17) 0.0204(17) 0.0016(13) 0.0146(15) 0.0005(13) N22P 0.0294(15) 0.0171(15) 0.0261(15) -0.0035(12) 0.0213(14) -0.0035(12) C23 0.039(2) 0.0211(19) 0.035(2) -0.0008(15) 0.0305(18) 0.0011(16) C24 0.039(2) 0.031(2) 0.045(2) 0.0010(17) 0.036(2) 0.0025(17) C25 0.0254(18) 0.029(2) 0.034(2) 0.0009(16) 0.0210(17) -0.0046(15) C26 0.0259(18) 0.0176(18) 0.0249(18) -0.0021(14) 0.0170(16) -0.0030(14) C31 0.0168(16) 0.0161(17) 0.0183(16) -0.0018(13) 0.0109(14) -0.0013(13) N32P 0.0169(13) 0.0145(14) 0.0195(14) 0.0006(11) 0.0108(12) 0.0019(11) C33 0.0261(18) 0.0145(17) 0.0257(18) 0.0027(13) 0.0170(16) 0.0020(14) C34 0.036(2) 0.023(2) 0.033(2) 0.0069(15) 0.0261(18) 0.0014(16) C35 0.030(2) 0.032(2) 0.039(2) 0.0002(16) 0.0277(18) -0.0025(16) C36 0.0228(11) 0.0227(11) 0.0258(11) -0.0006(8) 0.0157(8) 0.0007(8) C41 0.0177(16) 0.0134(17) 0.0172(16) -0.0024(12) 0.0107(14) 0.0002(13) N42P 0.0205(14) 0.0124(14) 0.0183(14) -0.0027(11) 0.0128(12) -0.0003(11) C43 0.0268(18) 0.0130(17) 0.0191(17) 0.0002(13) 0.0145(15) 0.0029(14) C44 0.0200(17) 0.025(2) 0.0196(17) 0.0019(14) 0.0100(15) 0.0098(14) C45 0.0150(16) 0.029(2) 0.0265(19) -0.0040(15) 0.0107(15) 0.0009(14) C51 0.0149(15) 0.0137(17) 0.0170(16) 0.0032(12) 0.0095(14) 0.0023(13) N52P 0.0170(14) 0.0140(14) 0.0249(15) -0.0025(11) 0.0117(12) -0.0004(11) C53 0.0189(17) 0.0172(18) 0.033(2) -0.0064(14) 0.0136(16) -0.0033(14) C54 0.0173(17) 0.025(2) 0.037(2) -0.0061(16) 0.0150(16) -0.0023(15) C55 0.0224(18) 0.0224(19) 0.036(2) -0.0036(15) 0.0198(17) 0.0011(15) C56 0.0232(18) 0.0176(18) 0.0265(18) -0.0044(14) 0.0158(16) 0.0000(14) C61 0.0166(16) 0.0168(17) 0.0205(17) 0.0009(13) 0.0116(14) 0.0052(13) N62P 0.0242(15) 0.0243(16) 0.0223(15) 0.0031(12) 0.0158(13) 0.0055(12) C63 0.0267(19) 0.033(2) 0.0228(18) 0.0020(15) 0.0164(16) 0.0069(16) C64 0.0269(19) 0.031(2) 0.0218(18) -0.0047(15) 0.0126(16) 0.0050(16) C65 0.0232(18) 0.0204(19) 0.0250(18) -0.0054(14) 0.0110(16) -0.0018(14) C66 0.0193(16) 0.0199(18) 0.0211(17) -0.0007(14) 0.0113(15) -0.0013(14) C71 0.0162(16) 0.0185(18) 0.0219(17) 0.0012(13) 0.0137(15) -0.0010(13) N72P 0.0207(14) 0.0162(15) 0.0222(15) -0.0041(11) 0.0116(13) 0.0007(12) C73 0.0302(19) 0.0226(19) 0.0279(19) -0.0058(15) 0.0192(17) 0.0001(15) C74 0.0286(19) 0.045(2) 0.0202(18) -0.0082(16) 0.0154(17) -0.0062(17) C75 0.0238(18) 0.045(2) 0.0220(19) 0.0092(16) 0.0148(16) 0.0079(17) C76 0.0249(18) 0.025(2) 0.0273(19) 0.0053(15) 0.0181(16) 0.0068(15) C81 0.0167(16) 0.0114(17) 0.0188(16) -0.0018(12) 0.0096(14) -0.0024(13) N82P 0.0212(14) 0.0134(14) 0.0215(14) 0.0001(11) 0.0125(12) 0.0000(11) C83 0.0223(17) 0.0147(17) 0.0205(17) 0.0006(13) 0.0123(15) 0.0006(13) C84 0.0288(19) 0.0197(19) 0.0259(18) 0.0016(14) 0.0171(16) -0.0028(15) C85 0.0242(18) 0.0237(19) 0.0324(19) -0.0024(15) 0.0211(17) -0.0025(15) C86 0.0231(17) 0.0178(18) 0.0276(18) 0.0017(14) 0.0174(16) 0.0026(14) C91 0.0229(17) 0.0162(18) 0.0209(17) 0.0031(13) 0.0143(15) 0.0018(14) N92P 0.0367(17) 0.0182(15) 0.0332(16) -0.0036(12) 0.0272(15) -0.0038(13) C93 0.062(3) 0.022(2) 0.056(2) -0.0065(18) 0.052(2) -0.0034(18) C94 0.052(2) 0.031(2) 0.059(3) 0.0002(19) 0.049(2) 0.0003(19) C95 0.034(2) 0.032(2) 0.039(2) -0.0009(17) 0.0275(19) -0.0050(17) C96 0.0298(19) 0.0209(19) 0.0275(19) -0.0011(14) 0.0202(17) -0.0027(15) C101 0.0160(17) 0.026(2) 0.0281(19) -0.0058(15) 0.0120(16) 0.0030(14) N102 0.0278(16) 0.0327(18) 0.0276(16) -0.0066(13) 0.0170(14) 0.0031(13) C103 0.032(2) 0.054(3) 0.028(2) -0.0057(19) 0.0171(18) 0.009(2) C104 0.022(2) 0.063(3) 0.030(2) -0.024(2) 0.0090(18) -0.0019(19) C105 0.0217(19) 0.037(2) 0.049(2) -0.0221(19) 0.0167(19) -0.0066(17) C106 0.0186(17) 0.030(2) 0.039(2) -0.0119(17) 0.0181(17) -0.0042(15) C111 0.0188(16) 0.0129(17) 0.0200(16) 0.0014(13) 0.0128(14) -0.0002(13) N112 0.0184(14) 0.0130(14) 0.0234(14) -0.0002(11) 0.0132(12) 0.0002(11) C113 0.0170(16) 0.0171(18) 0.0236(17) -0.0031(13) 0.0112(15) -0.0025(13) C114 0.0155(16) 0.0225(18) 0.0232(17) -0.0008(14) 0.0119(15) -0.0016(14) C115 0.0220(17) 0.0213(18) 0.0295(18) -0.0032(14) 0.0184(16) 0.0038(14) C116 0.0215(17) 0.0136(17) 0.0297(19) -0.0053(14) 0.0159(16) -0.0013(13) C121 0.0184(16) 0.0133(17) 0.0190(16) -0.0038(13) 0.0110(14) -0.0005(13) N122 0.0214(14) 0.0138(14) 0.0217(14) 0.0000(11) 0.0128(13) 0.0009(11) C123 0.0283(19) 0.0195(19) 0.0211(18) 0.0008(14) 0.0140(16) 0.0034(15) C124 0.030(2) 0.0220(19) 0.0259(19) 0.0040(14) 0.0165(17) 0.0078(15) C125 0.0183(17) 0.030(2) 0.0298(19) -0.0058(16) 0.0134(16) 0.0017(15) C126 0.0201(17) 0.0157(18) 0.0314(19) -0.0036(14) 0.0168(16) -0.0017(14) C1S 0.043(3) 0.064(3) 0.038(2) -0.013(2) 0.024(2) -0.005(2) C2S 0.059(3) 0.039(3) 0.034(2) -0.0009(18) 0.026(2) 0.001(2) C3S 0.045(3) 0.027(2) 0.039(2) -0.0091(18) 0.016(2) 0.0047(19) C4S 0.059(3) 0.027(2) 0.065(3) -0.016(2) 0.043(3) -0.005(2) C5S 0.069(3) 0.038(3) 0.046(3) -0.001(2) 0.040(3) 0.005(2) C6S 0.048(3) 0.056(3) 0.030(2) 0.000(2) 0.017(2) 0.015(2) C7S 0.070(4) 0.127(5) 0.073(4) -0.028(4) 0.051(3) -0.028(4) C8S 0.043(2) 0.028(2) 0.038(2) -0.0017(17) 0.025(2) 0.0043(18) C9S 0.039(2) 0.024(2) 0.065(3) 0.0029(19) 0.039(2) -0.0018(17) C10S 0.050(3) 0.032(2) 0.054(3) 0.005(2) 0.034(2) 0.005(2) C11S 0.059(3) 0.035(3) 0.051(3) 0.009(2) 0.033(3) 0.018(2) C12S 0.036(2) 0.041(3) 0.053(3) -0.011(2) 0.019(2) 0.005(2) C13S 0.035(2) 0.025(2) 0.052(3) -0.0053(17) 0.032(2) -0.0042(17) C14S 0.069(3) 0.047(3) 0.047(3) -0.011(2) 0.039(3) -0.007(2) C22S 0.067(3) 0.065(3) 0.050(3) 0.005(2) 0.035(3) 0.006(3) C23S 0.064(3) 0.041(3) 0.082(4) -0.001(3) 0.045(3) 0.018(2) C24S 0.053(3) 0.057(3) 0.072(4) -0.024(3) 0.034(3) -0.006(3) C25S 0.044(3) 0.055(3) 0.067(3) -0.014(3) 0.028(3) -0.013(2) C26S 0.041(3) 0.050(3) 0.067(3) 0.017(2) 0.034(3) 0.003(2) C27S 0.054(3) 0.058(3) 0.067(3) 0.015(2) 0.046(3) 0.011(2) C28S 0.113(5) 0.088(5) 0.061(4) -0.015(3) 0.046(4) -0.002(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 P1 O1 1.476(2) . ? P1 N3 1.649(3) . ? P1 N1 1.650(2) . ? P1 N2 1.655(3) . ? P2 O2 1.476(2) . ? P2 N6 1.644(2) . ? P2 N4 1.646(3) . ? P2 N5 1.654(2) . ? P3 O3 1.474(2) . ? P3 N7 1.642(3) . ? P3 N8 1.647(3) . ? P3 N9 1.655(3) . ? P4 O4 1.477(2) . ? P4 N12 1.640(3) . ? P4 N10 1.640(3) . ? P4 N11 1.655(3) . ? N1 C11 1.387(4) . ? N1 H1 0.8800 . ? N2 C21 1.395(4) . ? N2 H2 0.8800 . ? N3 C31 1.396(4) . ? N3 H3 0.8800 . ? N4 C41 1.392(4) . ? N4 H4 0.8800 . ? N5 C51 1.394(4) . ? N5 H5 0.8800 . ? N6 C61 1.401(4) . ? N6 H6 0.8800 . ? N7 C71 1.399(4) . ? N7 H7 0.8800 . ? N8 C81 1.398(4) . ? N8 H8 0.8800 . ? N9 C91 1.392(4) . ? N9 H9 0.8800 . ? N10 C101 1.399(4) . ? N10 H10 0.8800 . ? N11 C111 1.397(4) . ? N11 H11 0.8800 . ? N12 C121 1.395(4) . ? N12 H12 0.8800 . ? C11 N12P 1.335(4) . ? C11 C16 1.394(4) . ? N12P C13 1.341(4) . ? C46 C45 1.372(4) . ? C46 C41 1.388(4) . ? C46 H46 0.9500 . ? C13 C14 1.366(5) . ? C13 H13 0.9500 . ? C14 C15 1.387(5) . ? C14 H14 0.9500 . ? C15 C16 1.374(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 N22P 1.333(4) . ? C21 C26 1.395(4) . ? N22P C23 1.347(4) . ? C23 C24 1.370(5) . ? C23 H23 0.9500 . ? C24 C25 1.387(5) . ? C24 H24 0.9500 . ? C25 C26 1.371(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 N32P 1.337(4) . ? C31 C36 1.386(4) . ? N32P C33 1.347(4) . ? C33 C34 1.372(4) . ? C33 H33 0.9500 . ? C34 C35 1.394(5) . ? C34 H34 0.9500 . ? C35 C36 1.377(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 N42P 1.347(4) . ? N42P C43 1.351(4) . ? C43 C44 1.369(4) . ? C43 H43 0.9500 . ? C44 C45 1.391(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C51 N52P 1.325(4) . ? C51 C56 1.404(4) . ? N52P C53 1.342(4) . ? C53 C54 1.376(5) . ? C53 H53 0.9500 . ? C54 C55 1.389(5) . ? C54 H54 0.9500 . ? C55 C56 1.370(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 N62P 1.336(4) . ? C61 C66 1.405(4) . ? N62P C63 1.341(4) . ? C63 C64 1.369(5) . ? C63 H63 0.9500 . ? C64 C65 1.381(5) . ? C64 H64 0.9500 . ? C65 C66 1.374(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 N72P 1.333(4) . ? C71 C76 1.384(4) . ? N72P C73 1.342(4) . ? C73 C74 1.369(5) . ? C73 H73 0.9500 . ? C74 C75 1.392(5) . ? C74 H74 0.9500 . ? C75 C76 1.371(5) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 N82P 1.335(4) . ? C81 C86 1.392(4) . ? N82P C83 1.355(4) . ? C83 C84 1.365(4) . ? C83 H83 0.9500 . ? C84 C85 1.389(5) . ? C84 H84 0.9500 . ? C85 C86 1.380(4) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C91 N92P 1.332(4) . ? C91 C96 1.400(4) . ? N92P C93 1.340(4) . ? C93 C94 1.371(5) . ? C93 H93 0.9500 . ? C94 C95 1.381(5) . ? C94 H94 0.9500 . ? C95 C96 1.374(5) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C101 N102 1.341(4) . ? C101 C106 1.394(5) . ? N102 C103 1.338(4) . ? C103 C104 1.386(6) . ? C103 H103 0.9500 . ? C104 C105 1.384(6) . ? C104 H104 0.9500 . ? C105 C106 1.381(5) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C111 N112 1.332(4) . ? C111 C116 1.392(4) . ? N112 C113 1.339(4) . ? C113 C114 1.369(4) . ? C113 H113 0.9500 . ? C114 C115 1.387(4) . ? C114 H114 0.9500 . ? C115 C116 1.377(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 N122 1.338(4) . ? C121 C126 1.396(4) . ? N122 C123 1.351(4) . ? C123 C124 1.361(5) . ? C123 H123 0.9500 . ? C124 C125 1.395(5) . ? C124 H124 0.9500 . ? C125 C126 1.367(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C1S C2S 1.382(6) . ? C1S C6S 1.386(6) . ? C1S C7S 1.504(6) . ? C2S C3S 1.374(6) . ? C2S H2S 0.9500 . ? C3S C4S 1.382(6) . ? C3S H3S 0.9500 . ? C4S C5S 1.378(6) . ? C4S H4S 0.9500 . ? C5S C6S 1.372(6) . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? C7S H7S1 0.9800 . ? C7S H7S2 0.9800 . ? C7S H7S3 0.9800 . ? C8S C13S 1.387(5) . ? C8S C9S 1.398(5) . ? C8S C14S 1.479(5) . ? C9S C10S 1.346(5) . ? C9S H9S 0.9500 . ? C10S C11S 1.406(6) . ? C10S H10S 0.9500 . ? C11S C12S 1.359(6) . ? C11S H11S 0.9500 . ? C12S C13S 1.377(6) . ? C12S H12S 0.9500 . ? C13S H13S 0.9500 . ? C14S H14A 0.9800 . ? C14S H14B 0.9800 . ? C14S H14C 0.9800 . ? C15A C16A 1.3900 . ? C15A C20A 1.3900 . ? C15A C21A 1.5064 . ? C16A C17A 1.3900 . ? C16A H16A 0.9500 . ? C17A C18A 1.3900 . ? C17A H17A 0.9500 . ? C18A C19A 1.3900 . ? C18A H18A 0.9500 . ? C19A C20A 1.3900 . ? C19A H19A 0.9500 . ? C20A H20A 0.9500 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C15B C16B 1.3900 . ? C15B C20B 1.3900 . ? C15B C21B 1.4923 . ? C16B C17B 1.3900 . ? C16B H16B 0.9500 . ? C17B C18B 1.3900 . ? C17B H17B 0.9500 . ? C18B C19B 1.3900 . ? C18B H18B 0.9500 . ? C19B C20B 1.3900 . ? C19B H19B 0.9500 . ? C20B H20B 0.9500 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22S C27S 1.374(5) . ? C22S C23S 1.4090 . ? C22S C28S 1.479(6) . ? C23S C24S 1.323(6) . ? C23S H23S 0.9500 . ? C24S C25S 1.374(6) . ? C24S H24S 0.9500 . ? C25S C26S 1.355(6) . ? C25S H25S 0.9500 . ? C26S C27S 1.391(6) . ? C26S H26S 0.9500 . ? C27S H27S 0.9500 . ? C28S H28A 0.9800 . ? C28S H28B 0.9800 . ? C28S H28C 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 O1 P1 N3 109.92(13) . . ? O1 P1 N1 115.51(13) . . ? N3 P1 N1 109.67(13) . . ? O1 P1 N2 114.24(13) . . ? N3 P1 N2 104.78(13) . . ? N1 P1 N2 101.97(13) . . ? O2 P2 N6 112.54(13) . . ? O2 P2 N4 109.62(12) . . ? N6 P2 N4 110.81(13) . . ? O2 P2 N5 114.73(12) . . ? N6 P2 N5 103.39(13) . . ? N4 P2 N5 105.41(13) . . ? O3 P3 N7 115.70(13) . . ? O3 P3 N8 109.74(12) . . ? N7 P3 N8 109.64(13) . . ? O3 P3 N9 114.15(13) . . ? N7 P3 N9 101.62(13) . . ? N8 P3 N9 105.27(13) . . ? O4 P4 N12 109.58(13) . . ? O4 P4 N10 112.87(13) . . ? N12 P4 N10 111.51(13) . . ? O4 P4 N11 114.21(13) . . ? N12 P4 N11 105.05(13) . . ? N10 P4 N11 103.26(13) . . ? C11 N1 P1 127.5(2) . . ? C11 N1 H1 116.3 . . ? P1 N1 H1 116.3 . . ? C21 N2 P1 125.7(2) . . ? C21 N2 H2 117.1 . . ? P1 N2 H2 117.1 . . ? C31 N3 P1 129.3(2) . . ? C31 N3 H3 115.3 . . ? P1 N3 H3 115.3 . . ? C41 N4 P2 128.4(2) . . ? C41 N4 H4 115.8 . . ? P2 N4 H4 115.8 . . ? C51 N5 P2 126.5(2) . . ? C51 N5 H5 116.7 . . ? P2 N5 H5 116.7 . . ? C61 N6 P2 126.8(2) . . ? C61 N6 H6 116.6 . . ? P2 N6 H6 116.6 . . ? C71 N7 P3 126.5(2) . . ? C71 N7 H7 116.8 . . ? P3 N7 H7 116.8 . . ? C81 N8 P3 128.5(2) . . ? C81 N8 H8 115.7 . . ? P3 N8 H8 115.7 . . ? C91 N9 P3 126.1(2) . . ? C91 N9 H9 117.0 . . ? P3 N9 H9 117.0 . . ? C101 N10 P4 128.6(2) . . ? C101 N10 H10 115.7 . . ? P4 N10 H10 115.7 . . ? C111 N11 P4 125.7(2) . . ? C111 N11 H11 117.1 . . ? P4 N11 H11 117.1 . . ? C121 N12 P4 128.9(2) . . ? C121 N12 H12 115.6 . . ? P4 N12 H12 115.6 . . ? N12P C11 N1 117.9(3) . . ? N12P C11 C16 122.6(3) . . ? N1 C11 C16 119.4(3) . . ? C11 N12P C13 117.2(3) . . ? C45 C46 C41 118.6(3) . . ? C45 C46 H46 120.7 . . ? C41 C46 H46 120.7 . . ? N12P C13 C14 123.9(3) . . ? N12P C13 H13 118.0 . . ? C14 C13 H13 118.0 . . ? C13 C14 C15 118.4(3) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 118.9(3) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C15 C16 C11 118.9(3) . . ? C15 C16 H16 120.6 . . ? C11 C16 H16 120.6 . . ? N22P C21 C26 122.3(3) . . ? N22P C21 N2 115.3(3) . . ? C26 C21 N2 122.4(3) . . ? C21 N22P C23 117.5(3) . . ? N22P C23 C24 124.1(3) . . ? N22P C23 H23 118.0 . . ? C24 C23 H23 118.0 . . ? C23 C24 C25 117.5(3) . . ? C23 C24 H24 121.3 . . ? C25 C24 H24 121.3 . . ? C26 C25 C24 119.8(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C21 118.7(3) . . ? C25 C26 H26 120.7 . . ? C21 C26 H26 120.7 . . ? N32P C31 C36 123.0(3) . . ? N32P C31 N3 117.9(3) . . ? C36 C31 N3 119.2(3) . . ? C31 N32P C33 117.0(3) . . ? N32P C33 C34 124.2(3) . . ? N32P C33 H33 117.9 . . ? C34 C33 H33 117.9 . . ? C33 C34 C35 117.8(3) . . ? C33 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? C36 C35 C34 119.1(3) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C31 118.9(3) . . ? C35 C36 H36 120.5 . . ? C31 C36 H36 120.5 . . ? N42P C41 C46 123.3(3) . . ? N42P C41 N4 117.7(3) . . ? C46 C41 N4 119.0(3) . . ? C41 N42P C43 116.3(3) . . ? N42P C43 C44 124.3(3) . . ? N42P C43 H43 117.8 . . ? C44 C43 H43 117.8 . . ? C43 C44 C45 118.0(3) . . ? C43 C44 H44 121.0 . . ? C45 C44 H44 121.0 . . ? C46 C45 C44 119.5(3) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? N52P C51 N5 115.5(3) . . ? N52P C51 C56 122.4(3) . . ? N5 C51 C56 122.1(3) . . ? C51 N52P C53 117.8(3) . . ? N52P C53 C54 124.2(3) . . ? N52P C53 H53 117.9 . . ? C54 C53 H53 117.9 . . ? C53 C54 C55 117.2(3) . . ? C53 C54 H54 121.4 . . ? C55 C54 H54 121.4 . . ? C56 C55 C54 120.0(3) . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 118.4(3) . . ? C55 C56 H56 120.8 . . ? C51 C56 H56 120.8 . . ? N62P C61 N6 114.9(3) . . ? N62P C61 C66 123.2(3) . . ? N6 C61 C66 121.9(3) . . ? C61 N62P C63 116.6(3) . . ? N62P C63 C64 124.5(3) . . ? N62P C63 H63 117.8 . . ? C64 C63 H63 117.8 . . ? C63 C64 C65 118.1(3) . . ? C63 C64 H64 121.0 . . ? C65 C64 H64 121.0 . . ? C66 C65 C64 119.7(3) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C61 117.8(3) . . ? C65 C66 H66 121.1 . . ? C61 C66 H66 121.1 . . ? N72P C71 C76 123.5(3) . . ? N72P C71 N7 116.7(3) . . ? C76 C71 N7 119.8(3) . . ? C71 N72P C73 116.7(3) . . ? N72P C73 C74 124.1(3) . . ? N72P C73 H73 118.0 . . ? C74 C73 H73 118.0 . . ? C73 C74 C75 118.1(3) . . ? C73 C74 H74 120.9 . . ? C75 C74 H74 120.9 . . ? C76 C75 C74 118.8(3) . . ? C76 C75 H75 120.6 . . ? C74 C75 H75 120.6 . . ? C75 C76 C71 118.7(3) . . ? C75 C76 H76 120.6 . . ? C71 C76 H76 120.6 . . ? N82P C81 C86 123.4(3) . . ? N82P C81 N8 118.1(3) . . ? C86 C81 N8 118.4(3) . . ? C81 N82P C83 116.7(3) . . ? N82P C83 C84 124.3(3) . . ? N82P C83 H83 117.9 . . ? C84 C83 H83 117.9 . . ? C83 C84 C85 117.8(3) . . ? C83 C84 H84 121.1 . . ? C85 C84 H84 121.1 . . ? C86 C85 C84 119.8(3) . . ? C86 C85 H85 120.1 . . ? C84 C85 H85 120.1 . . ? C85 C86 C81 118.0(3) . . ? C85 C86 H86 121.0 . . ? C81 C86 H86 121.0 . . ? N92P C91 N9 115.7(3) . . ? N92P C91 C96 122.0(3) . . ? N9 C91 C96 122.3(3) . . ? C91 N92P C93 117.8(3) . . ? N92P C93 C94 124.1(3) . . ? N92P C93 H93 118.0 . . ? C94 C93 H93 118.0 . . ? C93 C94 C95 117.7(3) . . ? C93 C94 H94 121.2 . . ? C95 C94 H94 121.2 . . ? C96 C95 C94 119.7(3) . . ? C96 C95 H95 120.1 . . ? C94 C95 H95 120.1 . . ? C95 C96 C91 118.6(3) . . ? C95 C96 H96 120.7 . . ? C91 C96 H96 120.7 . . ? N102 C101 C106 123.4(3) . . ? N102 C101 N10 114.0(3) . . ? C106 C101 N10 122.6(3) . . ? C103 N102 C101 117.1(3) . . ? N102 C103 C104 124.0(4) . . ? N102 C103 H103 118.0 . . ? C104 C103 H103 118.0 . . ? C105 C104 C103 117.6(3) . . ? C105 C104 H104 121.2 . . ? C103 C104 H104 121.2 . . ? C106 C105 C104 120.0(4) . . ? C106 C105 H105 120.0 . . ? C104 C105 H105 120.0 . . ? C105 C106 C101 117.8(4) . . ? C105 C106 H106 121.1 . . ? C101 C106 H106 121.1 . . ? N112 C111 C116 122.2(3) . . ? N112 C111 N11 115.2(3) . . ? C116 C111 N11 122.6(3) . . ? C111 N112 C113 118.0(3) . . ? N112 C113 C114 124.0(3) . . ? N112 C113 H113 118.0 . . ? C114 C113 H113 118.0 . . ? C113 C114 C115 117.5(3) . . ? C113 C114 H114 121.2 . . ? C115 C114 H114 121.2 . . ? C116 C115 C114 119.7(3) . . ? C116 C115 H115 120.1 . . ? C114 C115 H115 120.1 . . ? C115 C116 C111 118.5(3) . . ? C115 C116 H116 120.7 . . ? C111 C116 H116 120.7 . . ? N122 C121 N12 117.8(3) . . ? N122 C121 C126 123.0(3) . . ? N12 C121 C126 119.2(3) . . ? C121 N122 C123 116.7(3) . . ? N122 C123 C124 124.2(3) . . ? N122 C123 H123 117.9 . . ? C124 C123 H123 117.9 . . ? C123 C124 C125 118.2(3) . . ? C123 C124 H124 120.9 . . ? C125 C124 H124 120.9 . . ? C126 C125 C124 119.1(3) . . ? C126 C125 H125 120.4 . . ? C124 C125 H125 120.4 . . ? C125 C126 C121 118.7(3) . . ? C125 C126 H126 120.6 . . ? C121 C126 H126 120.6 . . ? C2S C1S C6S 117.8(4) . . ? C2S C1S C7S 121.1(4) . . ? C6S C1S C7S 121.1(4) . . ? C3S C2S C1S 121.4(4) . . ? C3S C2S H2S 119.3 . . ? C1S C2S H2S 119.3 . . ? C2S C3S C4S 120.0(4) . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C5S C4S C3S 119.4(4) . . ? C5S C4S H4S 120.3 . . ? C3S C4S H4S 120.3 . . ? C6S C5S C4S 120.1(4) . . ? C6S C5S H5S 120.0 . . ? C4S C5S H5S 120.0 . . ? C5S C6S C1S 121.3(4) . . ? C5S C6S H6S 119.3 . . ? C1S C6S H6S 119.3 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C13S C8S C9S 117.4(4) . . ? C13S C8S C14S 122.0(4) . . ? C9S C8S C14S 120.6(4) . . ? C10S C9S C8S 121.5(4) . . ? C10S C9S H9S 119.3 . . ? C8S C9S H9S 119.3 . . ? C9S C10S C11S 121.1(4) . . ? C9S C10S H10S 119.5 . . ? C11S C10S H10S 119.5 . . ? C12S C11S C10S 117.5(4) . . ? C12S C11S H11S 121.2 . . ? C10S C11S H11S 121.2 . . ? C11S C12S C13S 122.0(4) . . ? C11S C12S H12S 119.0 . . ? C13S C12S H12S 119.0 . . ? C12S C13S C8S 120.5(4) . . ? C12S C13S H13S 119.7 . . ? C8S C13S H13S 119.7 . . ? C8S C14S H14A 109.5 . . ? C8S C14S H14B 109.5 . . ? H14A C14S H14B 109.5 . . ? C8S C14S H14C 109.5 . . ? H14A C14S H14C 109.5 . . ? H14B C14S H14C 109.5 . . ? C16A C15A C20A 120.0 . . ? C16A C15A C21A 119.8 . . ? C20A C15A C21A 120.2 . . ? C15A C16A C17A 120.0 . . ? C15A C16A H16A 120.0 . . ? C17A C16A H16A 120.0 . . ? C18A C17A C16A 120.0 . . ? C18A C17A H17A 120.0 . . ? C16A C17A H17A 120.0 . . ? C17A C18A C19A 120.0 . . ? C17A C18A H18A 120.0 . . ? C19A C18A H18A 120.0 . . ? C18A C19A C20A 120.0 . . ? C18A C19A H19A 120.0 . . ? C20A C19A H19A 120.0 . . ? C19A C20A C15A 120.0 . . ? C19A C20A H20A 120.0 . . ? C15A C20A H20A 120.0 . . ? C15A C21A H21A 109.5 . . ? C15A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C15A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C16B C15B C20B 120.0 . . ? C16B C15B C21B 118.5 . . ? C20B C15B C21B 121.5 . . ? C15B C16B C17B 120.0 . . ? C15B C16B H16B 120.0 . . ? C17B C16B H16B 120.0 . . ? C18B C17B C16B 120.0 . . ? C18B C17B H17B 120.0 . . ? C16B C17B H17B 120.0 . . ? C17B C18B C19B 120.0 . . ? C17B C18B H18B 120.0 . . ? C19B C18B H18B 120.0 . . ? C18B C19B C20B 120.0 . . ? C18B C19B H19B 120.0 . . ? C20B C19B H19B 120.0 . . ? C19B C20B C15B 120.0 . . ? C19B C20B H20B 120.0 . . ? C15B C20B H20B 120.0 . . ? C15B C21B H21D 109.5 . . ? C15B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C15B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C27S C22S C23S 116.8(3) . . ? C27S C22S C28S 120.2(4) . . ? C23S C22S C28S 122.9(3) . . ? C24S C23S C22S 123.2(3) . . ? C24S C23S H23S 118.4 . . ? C22S C23S H23S 118.4 . . ? C23S C24S C25S 118.9(5) . . ? C23S C24S H24S 120.5 . . ? C25S C24S H24S 120.5 . . ? C26S C25S C24S 120.9(5) . . ? C26S C25S H25S 119.5 . . ? C24S C25S H25S 119.5 . . ? C25S C26S C27S 119.9(4) . . ? C25S C26S H26S 120.0 . . ? C27S C26S H26S 120.0 . . ? C22S C27S C26S 120.2(4) . . ? C22S C27S H27S 119.9 . . ? C26S C27S H27S 119.9 . . ? C22S C28S H28A 109.5 . . ? C22S C28S H28B 109.5 . . ? H28A C28S H28B 109.5 . . ? C22S C28S H28C 109.5 . . ? H28A C28S H28C 109.5 . . ? H28B C28S H28C 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 O1 P1 N1 C11 -54.8(3) . . . . ? N3 P1 N1 C11 70.1(3) . . . . ? N2 P1 N1 C11 -179.3(3) . . . . ? O1 P1 N2 C21 -60.9(3) . . . . ? N3 P1 N2 C21 178.8(2) . . . . ? N1 P1 N2 C21 64.4(3) . . . . ? O1 P1 N3 C31 163.5(2) . . . . ? N1 P1 N3 C31 35.5(3) . . . . ? N2 P1 N3 C31 -73.3(3) . . . . ? O2 P2 N4 C41 161.0(2) . . . . ? N6 P2 N4 C41 36.2(3) . . . . ? N5 P2 N4 C41 -75.0(3) . . . . ? O2 P2 N5 C51 -52.9(3) . . . . ? N6 P2 N5 C51 70.1(3) . . . . ? N4 P2 N5 C51 -173.6(2) . . . . ? O2 P2 N6 C61 -43.5(3) . . . . ? N4 P2 N6 C61 79.6(3) . . . . ? N5 P2 N6 C61 -167.9(2) . . . . ? O3 P3 N7 C71 55.9(3) . . . . ? N8 P3 N7 C71 -68.9(3) . . . . ? N9 P3 N7 C71 -179.9(2) . . . . ? O3 P3 N8 C81 -161.9(2) . . . . ? N7 P3 N8 C81 -33.8(3) . . . . ? N9 P3 N8 C81 74.8(3) . . . . ? O3 P3 N9 C91 60.8(3) . . . . ? N7 P3 N9 C91 -64.5(3) . . . . ? N8 P3 N9 C91 -178.8(2) . . . . ? O4 P4 N10 C101 42.7(3) . . . . ? N12 P4 N10 C101 -81.2(3) . . . . ? N11 P4 N10 C101 166.5(3) . . . . ? O4 P4 N11 C111 53.4(3) . . . . ? N12 P4 N11 C111 173.5(2) . . . . ? N10 P4 N11 C111 -69.6(3) . . . . ? O4 P4 N12 C121 -162.7(2) . . . . ? N10 P4 N12 C121 -37.0(3) . . . . ? N11 P4 N12 C121 74.2(3) . . . . ? P1 N1 C11 N12P 20.2(4) . . . . ? P1 N1 C11 C16 -161.1(2) . . . . ? N1 C11 N12P C13 177.9(3) . . . . ? C16 C11 N12P C13 -0.8(5) . . . . ? C11 N12P C13 C14 -0.6(5) . . . . ? N12P C13 C14 C15 1.4(5) . . . . ? C13 C14 C15 C16 -0.8(5) . . . . ? C14 C15 C16 C11 -0.4(5) . . . . ? N12P C11 C16 C15 1.3(5) . . . . ? N1 C11 C16 C15 -177.4(3) . . . . ? P1 N2 C21 N22P -171.6(2) . . . . ? P1 N2 C21 C26 8.4(4) . . . . ? C26 C21 N22P C23 -2.5(4) . . . . ? N2 C21 N22P C23 177.5(3) . . . . ? C21 N22P C23 C24 -0.6(5) . . . . ? N22P C23 C24 C25 2.8(5) . . . . ? C23 C24 C25 C26 -1.8(5) . . . . ? C24 C25 C26 C21 -1.0(5) . . . . ? N22P C21 C26 C25 3.3(5) . . . . ? N2 C21 C26 C25 -176.7(3) . . . . ? P1 N3 C31 N32P 17.7(4) . . . . ? P1 N3 C31 C36 -162.2(2) . . . . ? C36 C31 N32P C33 1.5(4) . . . . ? N3 C31 N32P C33 -178.5(3) . . . . ? C31 N32P C33 C34 -0.5(5) . . . . ? N32P C33 C34 C35 -0.8(5) . . . . ? C33 C34 C35 C36 1.0(5) . . . . ? C34 C35 C36 C31 0.0(5) . . . . ? N32P C31 C36 C35 -1.3(5) . . . . ? N3 C31 C36 C35 178.7(3) . . . . ? C45 C46 C41 N42P -1.9(5) . . . . ? C45 C46 C41 N4 178.0(3) . . . . ? P2 N4 C41 N42P 21.0(4) . . . . ? P2 N4 C41 C46 -158.9(2) . . . . ? C46 C41 N42P C43 1.4(4) . . . . ? N4 C41 N42P C43 -178.5(2) . . . . ? C41 N42P C43 C44 0.0(4) . . . . ? N42P C43 C44 C45 -0.9(5) . . . . ? C41 C46 C45 C44 0.9(5) . . . . ? C43 C44 C45 C46 0.4(5) . . . . ? P2 N5 C51 N52P -169.6(2) . . . . ? P2 N5 C51 C56 10.6(4) . . . . ? N5 C51 N52P C53 178.6(3) . . . . ? C56 C51 N52P C53 -1.6(4) . . . . ? C51 N52P C53 C54 0.3(5) . . . . ? N52P C53 C54 C55 0.7(5) . . . . ? C53 C54 C55 C56 -0.6(5) . . . . ? C54 C55 C56 C51 -0.6(5) . . . . ? N52P C51 C56 C55 1.8(5) . . . . ? N5 C51 C56 C55 -178.5(3) . . . . ? P2 N6 C61 N62P 168.2(2) . . . . ? P2 N6 C61 C66 -11.8(4) . . . . ? N6 C61 N62P C63 -178.3(3) . . . . ? C66 C61 N62P C63 1.7(4) . . . . ? C61 N62P C63 C64 -0.6(5) . . . . ? N62P C63 C64 C65 -0.6(5) . . . . ? C63 C64 C65 C66 0.7(5) . . . . ? C64 C65 C66 C61 0.3(5) . . . . ? N62P C61 C66 C65 -1.6(5) . . . . ? N6 C61 C66 C65 178.4(3) . . . . ? P3 N7 C71 N72P -14.3(4) . . . . ? P3 N7 C71 C76 165.7(2) . . . . ? C76 C71 N72P C73 3.1(5) . . . . ? N7 C71 N72P C73 -176.9(3) . . . . ? C71 N72P C73 C74 -0.6(5) . . . . ? N72P C73 C74 C75 -1.9(5) . . . . ? C73 C74 C75 C76 1.8(5) . . . . ? C74 C75 C76 C71 0.6(5) . . . . ? N72P C71 C76 C75 -3.2(5) . . . . ? N7 C71 C76 C75 176.9(3) . . . . ? P3 N8 C81 N82P -20.2(4) . . . . ? P3 N8 C81 C86 160.4(2) . . . . ? C86 C81 N82P C83 -1.5(4) . . . . ? N8 C81 N82P C83 179.2(3) . . . . ? C81 N82P C83 C84 0.9(4) . . . . ? N82P C83 C84 C85 0.3(5) . . . . ? C83 C84 C85 C86 -1.1(5) . . . . ? C84 C85 C86 C81 0.6(5) . . . . ? N82P C81 C86 C85 0.7(5) . . . . ? N8 C81 C86 C85 -179.9(3) . . . . ? P3 N9 C91 N92P 173.6(2) . . . . ? P3 N9 C91 C96 -5.4(4) . . . . ? N9 C91 N92P C93 -178.4(3) . . . . ? C96 C91 N92P C93 0.6(5) . . . . ? C91 N92P C93 C94 0.7(5) . . . . ? N92P C93 C94 C95 -1.5(6) . . . . ? C93 C94 C95 C96 0.9(5) . . . . ? C94 C95 C96 C91 0.3(5) . . . . ? N92P C91 C96 C95 -1.1(5) . . . . ? N9 C91 C96 C95 177.9(3) . . . . ? P4 N10 C101 N102 -169.8(2) . . . . ? P4 N10 C101 C106 10.4(4) . . . . ? C106 C101 N102 C103 -0.9(5) . . . . ? N10 C101 N102 C103 179.4(3) . . . . ? C101 N102 C103 C104 0.3(5) . . . . ? N102 C103 C104 C105 0.4(6) . . . . ? C103 C104 C105 C106 -0.7(5) . . . . ? C104 C105 C106 C101 0.3(5) . . . . ? N102 C101 C106 C105 0.6(5) . . . . ? N10 C101 C106 C105 -179.7(3) . . . . ? P4 N11 C111 N112 165.8(2) . . . . ? P4 N11 C111 C116 -15.2(4) . . . . ? C116 C111 N112 C113 2.6(4) . . . . ? N11 C111 N112 C113 -178.3(3) . . . . ? C111 N112 C113 C114 -0.8(5) . . . . ? N112 C113 C114 C115 -1.0(5) . . . . ? C113 C114 C115 C116 0.9(5) . . . . ? C114 C115 C116 C111 0.9(5) . . . . ? N112 C111 C116 C115 -2.7(5) . . . . ? N11 C111 C116 C115 178.3(3) . . . . ? P4 N12 C121 N122 -18.7(4) . . . . ? P4 N12 C121 C126 161.6(2) . . . . ? N12 C121 N122 C123 178.4(3) . . . . ? C126 C121 N122 C123 -1.9(4) . . . . ? C121 N122 C123 C124 0.7(5) . . . . ? N122 C123 C124 C125 0.6(5) . . . . ? C123 C124 C125 C126 -0.7(5) . . . . ? C124 C125 C126 C121 -0.4(5) . . . . ? N122 C121 C126 C125 1.7(5) . . . . ? N12 C121 C126 C125 -178.5(3) . . . . ? C6S C1S C2S C3S 0.0(6) . . . . ? C7S C1S C2S C3S 179.9(4) . . . . ? C1S C2S C3S C4S 0.7(6) . . . . ? C2S C3S C4S C5S -1.1(6) . . . . ? C3S C4S C5S C6S 0.8(6) . . . . ? C4S C5S C6S C1S 0.0(6) . . . . ? C2S C1S C6S C5S -0.4(6) . . . . ? C7S C1S C6S C5S 179.8(4) . . . . ? C13S C8S C9S C10S 1.0(6) . . . . ? C14S C8S C9S C10S -179.3(4) . . . . ? C8S C9S C10S C11S 0.5(6) . . . . ? C9S C10S C11S C12S -1.2(6) . . . . ? C10S C11S C12S C13S 0.3(6) . . . . ? C11S C12S C13S C8S 1.2(6) . . . . ? C9S C8S C13S C12S -1.8(5) . . . . ? C14S C8S C13S C12S 178.4(4) . . . . ? C20A C15A C16A C17A 0.0 . . . . ? C21A C15A C16A C17A 179.4 . . . . ? C15A C16A C17A C18A 0.0 . . . . ? C16A C17A C18A C19A 0.0 . . . . ? C17A C18A C19A C20A 0.0 . . . . ? C18A C19A C20A C15A 0.0 . . . . ? C16A C15A C20A C19A 0.0 . . . . ? C21A C15A C20A C19A -179.4 . . . . ? C20B C15B C16B C17B 0.0 . . . . ? C21B C15B C16B C17B 179.0 . . . . ? C15B C16B C17B C18B 0.0 . . . . ? C16B C17B C18B C19B 0.0 . . . . ? C17B C18B C19B C20B 0.0 . . . . ? C18B C19B C20B C15B 0.0 . . . . ? C16B C15B C20B C19B 0.0 . . . . ? C21B C15B C20B C19B -179.0 . . . . ? C27S C22S C23S C24S 0.7(4) . . . . ? C28S C22S C23S C24S -178.4(5) . . . . ? C22S C23S C24S C25S 1.1(6) . . . . ? C23S C24S C25S C26S -1.7(8) . . . . ? C24S C25S C26S C27S 0.5(7) . . . . ? C23S C22S C27S C26S -2.0(5) . . . . ? C28S C22S C27S C26S 177.1(5) . . . . ? C25S C26S C27S C22S 1.4(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 N52P 0.88 1.99 2.853(4) 167.8 . N2 H2 N42P 0.88 2.16 3.035(4) 172.9 . N3 H3 O2 0.88 2.00 2.797(3) 149.5 2_645 N4 H4 O1 0.88 2.00 2.845(3) 159.7 2_655 N5 H5 N32P 0.88 2.10 2.977(3) 175.4 . N6 H6 N22P 0.88 1.98 2.853(4) 173.0 . N7 H7 N112 0.88 1.96 2.829(4) 168.5 . N8 H8 O4 0.88 2.02 2.776(3) 143.1 2 N9 H9 N122 0.88 2.19 3.058(4) 171.5 . N10 H10 N92P 0.88 1.99 2.867(4) 174.4 . N11 H11 N82P 0.88 2.10 2.981(4) 176.1 . N12 H12 O3 0.88 2.00 2.863(3) 166.1 2_545 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.698 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.060 data_ag039a _database_code_depnum_ccdc_archive 'CCDC 865263' #TrackingRef '- Compound2_new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H30 Ag3 N12 O2 P2 3+, (N O3 1-)3, (H2 O)3' _chemical_formula_sum 'C30 H36 Ag3 N15 O14 P2' _chemical_formula_weight 1216.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.0273(12) _cell_length_b 22.194(2) _cell_length_c 14.8103(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.846(5) _cell_angle_gamma 90.00 _cell_volume 4556.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 101 _cell_measurement_theta_min 4.11 _cell_measurement_theta_max 25.02 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 1.424 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Apex II' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 37399 _diffrn_reflns_av_R_equivalents 0.1091 _diffrn_reflns_av_sigmaI/netI 0.1368 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 22.51 _reflns_number_total 11649 _reflns_number_gt 7424 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The crystals were poorly diffracting, therefore the data at higher anlges (2-theta > 45 deg) were omitted. All non-hydrogen atoms were refined anisotropic with the exception of nitrate ions and water molecules, which were refined isotropic. A global SIMU restraint was applied for all N, C and O atoms. In addition the nitrate ions were refined with SAME restraints. H-atoms of disordered water molecules were not added to the model. ; _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^)+(0.1516P)^2^+2.8784P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.58(6) _refine_ls_number_reflns 11649 _refine_ls_number_parameters 1004 _refine_ls_number_restraints 865 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.2545 _refine_ls_wR_factor_gt 0.2212 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 0.997 _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 0.14287(14) 0.20575(8) 0.77170(14) 0.0570(6) Uani 1 1 d . . . Ag2 Ag 0.50159(13) 0.16532(9) 1.07746(13) 0.0543(6) Uani 1 1 d . . . Ag3 Ag 0.50831(16) 0.32858(10) 0.76381(14) 0.0663(7) Uani 1 1 d . . . Ag4 Ag 1.09614(13) 0.25580(8) 0.48926(14) 0.0544(5) Uani 1 1 d . . . Ag5 Ag 0.71888(15) 0.13490(9) 0.50295(13) 0.0601(6) Uani 1 1 d . . . Ag6 Ag 0.73337(13) 0.29369(9) 0.18037(13) 0.0545(5) Uani 1 1 d . . . P1 P 0.3042(5) 0.3390(3) 0.9968(5) 0.0470(17) Uani 1 1 d . . . P2 P 0.4577(5) 0.1184(3) 0.7573(4) 0.0466(18) Uani 1 1 d . . . P3 P 0.7852(4) 0.3457(3) 0.4980(4) 0.0429(16) Uani 1 1 d . . . P4 P 0.9274(4) 0.1189(3) 0.2745(4) 0.0417(15) Uani 1 1 d . . . O1 O 0.2764(12) 0.3894(9) 1.0510(13) 0.075(6) Uani 1 1 d . . . O2 O 0.4825(11) 0.0681(7) 0.7037(11) 0.050(4) Uani 1 1 d . . . O3 O 0.7578(11) 0.3983(7) 0.5490(11) 0.052(4) Uani 1 1 d . . . O4 O 0.9589(11) 0.0692(7) 0.2171(10) 0.047(4) Uani 1 1 d . . . N1 N 0.2157(12) 0.3044(9) 0.9305(14) 0.054(5) Uani 1 1 d U . . H1 H 0.2149 0.2657 0.9343 0.065 Uiso 1 1 calc R . . N2 N 0.3738(14) 0.3601(8) 0.9197(12) 0.047(5) Uani 1 1 d U . . H2 H 0.3585 0.3452 0.8658 0.057 Uiso 1 1 calc R . . N3 N 0.3634(13) 0.2833(8) 1.0566(13) 0.047(5) Uani 1 1 d U . . H3 H 0.4192 0.2752 1.0424 0.056 Uiso 1 1 calc R . . N4 N 0.3395(12) 0.1311(9) 0.7437(12) 0.049(5) Uani 1 1 d U . . H4 H 0.3210 0.1677 0.7336 0.058 Uiso 1 1 calc R . . N5 N 0.4877(12) 0.1115(8) 0.8703(12) 0.046(5) Uani 1 1 d U . . H5 H 0.4429 0.1155 0.9035 0.055 Uiso 1 1 calc R . . N6 N 0.5009(12) 0.1847(8) 0.7332(12) 0.045(5) Uani 1 1 d U . . H6 H 0.5302 0.2056 0.7781 0.054 Uiso 1 1 calc R . . N7 N 0.7413(14) 0.2827(8) 0.5232(14) 0.054(5) Uani 1 1 d U . . H7 H 0.7109 0.2624 0.4783 0.065 Uiso 1 1 calc R . . N8 N 0.9005(12) 0.3344(8) 0.5091(11) 0.039(4) Uani 1 1 d U . . H8 H 0.9183 0.2980 0.5224 0.047 Uiso 1 1 calc R . . N9 N 0.7504(13) 0.3508(9) 0.3843(11) 0.046(5) Uani 1 1 d U . . H9 H 0.7933 0.3423 0.3506 0.055 Uiso 1 1 calc R . . N10 N 0.8623(12) 0.1731(9) 0.2141(12) 0.046(5) Uani 1 1 d U . . H10 H 0.8058 0.1818 0.2261 0.055 Uiso 1 1 calc R . . N11 N 0.8570(13) 0.1013(8) 0.3481(12) 0.047(5) Uani 1 1 d U . . H11 H 0.8708 0.1178 0.4011 0.056 Uiso 1 1 calc R . . N12 N 1.0204(11) 0.1553(9) 0.3304(13) 0.051(5) Uani 1 1 d U . . H12 H 1.0221 0.1936 0.3226 0.062 Uiso 1 1 calc R . . C11 C 0.1425(14) 0.3303(11) 0.8693(16) 0.043(5) Uani 1 1 d U . . N12A N 0.0956(11) 0.2964(7) 0.8048(13) 0.038(4) Uani 1 1 d U . . C13 C 0.0237(17) 0.3212(12) 0.7434(16) 0.057(6) Uani 1 1 d U . . H13 H -0.0095 0.2968 0.6981 0.068 Uiso 1 1 calc R . . C14 C -0.0004(17) 0.3785(11) 0.7458(16) 0.049(6) Uani 1 1 d U . . H14 H -0.0457 0.3945 0.6996 0.059 Uiso 1 1 calc R . . C15 C 0.0415(17) 0.4148(12) 0.8169(18) 0.054(6) Uani 1 1 d U . . H15 H 0.0188 0.4537 0.8238 0.064 Uiso 1 1 calc R . . C16 C 0.1223(16) 0.3907(10) 0.8810(17) 0.044(6) Uani 1 1 d U . . H16 H 0.1576 0.4142 0.9263 0.053 Uiso 1 1 calc R . . C21 C 0.4558(16) 0.3999(10) 0.9318(18) 0.045(5) Uani 1 1 d U . . N22 N 0.5094(16) 0.3971(9) 0.8703(16) 0.062(6) Uani 1 1 d U . . C23 C 0.582(2) 0.4343(14) 0.873(3) 0.097(9) Uani 1 1 d U . . H23 H 0.6191 0.4366 0.8260 0.116 Uiso 1 1 calc R . . C24 C 0.602(3) 0.4727(17) 0.956(3) 0.106(10) Uani 1 1 d U . . H24 H 0.6596 0.4945 0.9653 0.127 Uiso 1 1 calc R . . C25 C 0.546(2) 0.4779(16) 1.017(3) 0.105(10) Uani 1 1 d U . . H25 H 0.5579 0.5046 1.0656 0.125 Uiso 1 1 calc R . . C26 C 0.467(2) 0.4417(13) 1.004(2) 0.076(8) Uani 1 1 d U . . H26 H 0.4211 0.4444 1.0432 0.091 Uiso 1 1 calc R . . C31 C 0.3368(16) 0.2483(12) 1.1253(14) 0.045(5) Uani 1 1 d U . . N32 N 0.3872(12) 0.1996(8) 1.1487(11) 0.035(4) Uani 1 1 d U . . C33 C 0.3588(19) 0.1683(15) 1.2111(19) 0.075(7) Uani 1 1 d U . . H33 H 0.3972 0.1350 1.2294 0.090 Uiso 1 1 calc R . . C34 C 0.282(2) 0.1752(17) 1.256(2) 0.091(9) Uani 1 1 d U . . H34 H 0.2644 0.1470 1.2967 0.109 Uiso 1 1 calc R . . C35 C 0.2345(19) 0.2260(15) 1.2356(18) 0.075(8) Uani 1 1 d U . . H35 H 0.1836 0.2351 1.2667 0.090 Uiso 1 1 calc R . . C36 C 0.2571(17) 0.2683(14) 1.1677(16) 0.067(8) Uani 1 1 d U . . H36 H 0.2241 0.3042 1.1533 0.081 Uiso 1 1 calc R . . C41 C 0.2686(14) 0.0891(10) 0.7470(15) 0.041(5) Uani 1 1 d U . . N42 N 0.1771(15) 0.1101(8) 0.7531(14) 0.055(5) Uani 1 1 d U . . C43 C 0.1052(17) 0.0728(12) 0.758(2) 0.070(7) Uani 1 1 d U . . H43 H 0.0446 0.0881 0.7629 0.084 Uiso 1 1 calc R . . C44 C 0.117(2) 0.0140(12) 0.755(2) 0.086(9) Uani 1 1 d U . . H44 H 0.0673 -0.0119 0.7626 0.103 Uiso 1 1 calc R . . C45 C 0.211(2) -0.0103(12) 0.738(2) 0.073(8) Uani 1 1 d U . . H45 H 0.2194 -0.0506 0.7246 0.088 Uiso 1 1 calc R . . C46 C 0.2826(17) 0.0288(11) 0.7442(16) 0.043(6) Uani 1 1 d U . . H46 H 0.3452 0.0144 0.7466 0.052 Uiso 1 1 calc R . . C51 C 0.5800(15) 0.0996(9) 0.9136(14) 0.034(5) Uani 1 1 d U . . N52 N 0.5985(11) 0.1138(8) 1.0068(12) 0.039(4) Uani 1 1 d U . . C53 C 0.6855(16) 0.1001(13) 1.0567(19) 0.070(7) Uani 1 1 d U . . H53 H 0.6981 0.1108 1.1181 0.084 Uiso 1 1 calc R . . C54 C 0.760(2) 0.0687(15) 1.015(2) 0.079(8) Uani 1 1 d U . . H54 H 0.8206 0.0609 1.0472 0.095 Uiso 1 1 calc R . . C55 C 0.734(2) 0.0511(14) 0.9243(18) 0.066(7) Uani 1 1 d U . . H55 H 0.7787 0.0285 0.8982 0.079 Uiso 1 1 calc R . . C56 C 0.6517(19) 0.0643(11) 0.8730(18) 0.052(6) Uani 1 1 d U . . H56 H 0.6389 0.0517 0.8124 0.063 Uiso 1 1 calc R . . C61 C 0.4940(16) 0.2090(12) 0.6482(15) 0.047(5) Uani 1 1 d U . . N62 N 0.5031(14) 0.2696(9) 0.6448(13) 0.057(5) Uani 1 1 d U . . C63 C 0.4877(18) 0.2996(14) 0.5609(17) 0.068(7) Uani 1 1 d U . . H63 H 0.4907 0.3414 0.5592 0.081 Uiso 1 1 calc R . . C64 C 0.4684(19) 0.2679(14) 0.4820(18) 0.068(8) Uani 1 1 d U . . H64 H 0.4579 0.2874 0.4257 0.081 Uiso 1 1 calc R . . C65 C 0.465(2) 0.2059(15) 0.4878(19) 0.073(7) Uani 1 1 d U . . H65 H 0.4570 0.1834 0.4342 0.088 Uiso 1 1 calc R . . C66 C 0.4722(17) 0.1764(13) 0.5691(16) 0.058(6) Uani 1 1 d U . . H66 H 0.4627 0.1350 0.5710 0.070 Uiso 1 1 calc R . . C71 C 0.7463(13) 0.2563(10) 0.6113(14) 0.035(5) Uani 1 1 d U . . N72 N 0.7314(14) 0.1983(9) 0.6160(12) 0.051(5) Uani 1 1 d U . . C73 C 0.743(2) 0.1736(14) 0.702(2) 0.075(7) Uani 1 1 d U . . H73 H 0.7375 0.1321 0.7085 0.090 Uiso 1 1 calc R . . C74 C 0.7616(19) 0.2087(15) 0.777(2) 0.078(8) Uani 1 1 d U . . H74 H 0.7697 0.1898 0.8337 0.093 Uiso 1 1 calc R . . C75 C 0.7695(19) 0.2694(12) 0.7756(18) 0.063(7) Uani 1 1 d U . . H75 H 0.7787 0.2923 0.8289 0.075 Uiso 1 1 calc R . . C76 C 0.7631(17) 0.2950(12) 0.6906(15) 0.055(6) Uani 1 1 d U . . H76 H 0.7694 0.3364 0.6842 0.066 Uiso 1 1 calc R . . C81 C 0.9767(15) 0.3747(10) 0.5003(15) 0.038(5) Uani 1 1 d U . . N82 N 1.0622(13) 0.3504(8) 0.5051(14) 0.055(5) Uani 1 1 d U . . C83 C 1.1437(18) 0.3895(14) 0.498(2) 0.076(8) Uani 1 1 d U . . H83 H 1.2046 0.3723 0.5003 0.091 Uiso 1 1 calc R . . C84 C 1.1343(17) 0.4526(13) 0.487(2) 0.072(8) Uani 1 1 d U . . H84 H 1.1846 0.4782 0.4780 0.086 Uiso 1 1 calc R . . C85 C 1.0423(19) 0.4716(11) 0.4910(18) 0.057(6) Uani 1 1 d U . . H85 H 1.0329 0.5130 0.4938 0.068 Uiso 1 1 calc R . . C86 C 0.961(2) 0.4355(11) 0.4915(17) 0.057(7) Uani 1 1 d U . . H86 H 0.8992 0.4518 0.4861 0.068 Uiso 1 1 calc R . . C91 C 0.6589(16) 0.3675(11) 0.3380(16) 0.041(6) Uani 1 1 d U . . N92 N 0.6394(13) 0.3461(10) 0.2561(12) 0.052(5) Uani 1 1 d U . . C93 C 0.5495(19) 0.3588(12) 0.2115(19) 0.061(7) Uani 1 1 d U . . H93 H 0.5359 0.3500 0.1495 0.073 Uiso 1 1 calc R . . C94 C 0.4785(18) 0.3837(16) 0.252(2) 0.077(8) Uani 1 1 d U . . H94 H 0.4148 0.3829 0.2234 0.092 Uiso 1 1 calc R . . C95 C 0.5012(18) 0.4089(14) 0.333(2) 0.071(7) Uani 1 1 d U . . H95 H 0.4571 0.4329 0.3576 0.085 Uiso 1 1 calc R . . C96 C 0.5958(17) 0.3984(12) 0.3826(18) 0.060(7) Uani 1 1 d U . . H96 H 0.6135 0.4120 0.4422 0.072 Uiso 1 1 calc R . . C101 C 0.9010(16) 0.2062(12) 0.1402(17) 0.056(6) Uani 1 1 d U . . N102 N 0.8460(14) 0.2547(10) 0.1171(14) 0.062(5) Uani 1 1 d U . . C103 C 0.8742(16) 0.2864(12) 0.0487(19) 0.062(7) Uani 1 1 d U . . H103 H 0.8398 0.3213 0.0305 0.074 Uiso 1 1 calc R . . C104 C 0.9516(17) 0.2715(11) 0.0018(17) 0.055(6) Uani 1 1 d U . . H104 H 0.9674 0.2949 -0.0459 0.066 Uiso 1 1 calc R . . C105 C 1.003(2) 0.2190(15) 0.032(2) 0.080(8) Uani 1 1 d U . . H105 H 1.0557 0.2070 0.0047 0.096 Uiso 1 1 calc R . . C106 C 0.9759(18) 0.1862(12) 0.1003(19) 0.061(7) Uani 1 1 d U . . H106 H 1.0078 0.1507 0.1196 0.073 Uiso 1 1 calc R . . C111 C 0.7785(19) 0.0637(11) 0.3366(17) 0.059(6) Uani 1 1 d U . . N112 N 0.7115(13) 0.0691(9) 0.3931(13) 0.057(5) Uani 1 1 d U . . C113 C 0.635(2) 0.0333(14) 0.382(2) 0.093(9) Uani 1 1 d U . . H113 H 0.5891 0.0397 0.4204 0.111 Uiso 1 1 calc R . . C114 C 0.619(2) -0.0108(14) 0.322(2) 0.087(8) Uani 1 1 d U . . H114 H 0.5657 -0.0363 0.3210 0.104 Uiso 1 1 calc R . . C115 C 0.684(2) -0.0179(13) 0.259(2) 0.074(8) Uani 1 1 d U . . H115 H 0.6715 -0.0466 0.2132 0.088 Uiso 1 1 calc R . . C116 C 0.7700(19) 0.0193(13) 0.2658(16) 0.061(7) Uani 1 1 d U . . H116 H 0.8159 0.0145 0.2272 0.073 Uiso 1 1 calc R . . C121 C 1.0985(17) 0.1291(11) 0.3906(16) 0.049(6) Uani 1 1 d U . . N122 N 1.1432(12) 0.1654(9) 0.4577(11) 0.044(4) Uani 1 1 d U . . C123 C 1.2191(18) 0.1411(12) 0.5107(17) 0.066(7) Uani 1 1 d U . . H123 H 1.2518 0.1650 0.5570 0.079 Uiso 1 1 calc R . . C124 C 1.255(2) 0.0791(14) 0.5017(19) 0.069(7) Uani 1 1 d U . . H124 H 1.3089 0.0635 0.5392 0.083 Uiso 1 1 calc R . . C125 C 1.204(2) 0.0479(10) 0.4352(18) 0.059(7) Uani 1 1 d U . . H125 H 1.2242 0.0088 0.4255 0.071 Uiso 1 1 calc R . . C126 C 1.1237(15) 0.0684(10) 0.3796(16) 0.039(5) Uani 1 1 d U . . H126 H 1.0876 0.0435 0.3367 0.047 Uiso 1 1 calc R . . N13 N 0.6002(13) 0.2617(9) 0.9633(12) 0.057(6) Uiso 1 1 d DU . . O5 O 0.5888(12) 0.2722(7) 1.0413(11) 0.070(5) Uiso 1 1 d DU . . O6 O 0.6579(18) 0.2922(13) 0.9316(18) 0.156(10) Uiso 1 1 d DU . . O7 O 0.5254(14) 0.2476(10) 0.9144(13) 0.103(7) Uiso 1 1 d DU . . N14 N 0.2649(10) 0.1400(6) 0.9566(10) 0.025(4) Uiso 1 1 d DU . . O8 O 0.3057(13) 0.0937(7) 0.9787(14) 0.091(6) Uiso 1 1 d DU . . O9 O 0.1885(12) 0.1524(9) 0.9762(15) 0.099(6) Uiso 1 1 d DU . . O10 O 0.3156(12) 0.1802(7) 0.9307(13) 0.078(5) Uiso 1 1 d DU . . N15 N 0.2885(12) 0.2959(8) 0.6871(11) 0.048(5) Uiso 1 1 d DU . . O11 O 0.2406(15) 0.2657(9) 0.6310(13) 0.106(7) Uiso 1 1 d DU . . O12 O 0.3135(15) 0.3460(8) 0.6739(14) 0.101(7) Uiso 1 1 d DU . . O13 O 0.3216(12) 0.2716(7) 0.7621(10) 0.065(5) Uiso 1 1 d DU . . N16 N 0.9726(11) 0.3212(7) 0.2887(12) 0.043(5) Uiso 1 1 d DU . . O14 O 1.0499(13) 0.3164(9) 0.2630(15) 0.098(7) Uiso 1 1 d DU . . O15 O 0.9291(14) 0.3663(8) 0.2611(15) 0.098(7) Uiso 1 1 d DU . . O16 O 0.9350(13) 0.2809(7) 0.3265(13) 0.081(6) Uiso 1 1 d DU . . N17 N 0.6467(11) 0.1967(7) 0.2926(10) 0.038(4) Uiso 1 1 d DU . . O17 O 0.6495(12) 0.1891(8) 0.2143(10) 0.071(5) Uiso 1 1 d DU . . O18 O 0.5795(15) 0.1891(12) 0.3319(16) 0.136(9) Uiso 1 1 d DU . . O19 O 0.7195(11) 0.2153(8) 0.3421(10) 0.063(4) Uiso 1 1 d DU . . N18 N 0.9463(12) 0.1663(7) 0.5739(11) 0.050(5) Uiso 1 1 d DU . . O20 O 0.9928(15) 0.1953(9) 0.6328(13) 0.105(7) Uiso 1 1 d DU . . O21 O 0.9215(13) 0.1146(7) 0.5813(12) 0.075(5) Uiso 1 1 d DU . . O22 O 0.9135(12) 0.1927(7) 0.5005(10) 0.063(5) Uiso 1 1 d DU . . O1S O 0.0018(14) 0.0405(9) 0.9812(14) 0.093(6) Uiso 1 1 d . . . O2S O 0.137(2) 0.4225(14) 0.190(2) 0.156(10) Uiso 1 1 d . . . O3S O 0.1512(11) 0.0317(7) 0.1240(11) 0.060(4) Uiso 1 1 d . . . O4S O 0.6316(15) 0.0377(9) 0.6061(14) 0.096(6) Uiso 1 1 d . . . O5S O 0.1759(19) 0.5255(11) 0.2879(18) 0.131(8) Uiso 1 1 d . . . O6S O 0.1322(17) -0.0584(10) 0.9857(16) 0.113(7) Uiso 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 0.0513(12) 0.0495(12) 0.0631(13) -0.0102(10) -0.0140(11) 0.0048(9) Ag2 0.0446(11) 0.0762(14) 0.0420(11) 0.0021(10) 0.0062(9) 0.0147(10) Ag3 0.0703(14) 0.0726(15) 0.0510(13) -0.0065(11) -0.0068(11) -0.0098(11) Ag4 0.0454(11) 0.0513(12) 0.0618(13) -0.0108(10) -0.0064(10) 0.0066(9) Ag5 0.0611(13) 0.0650(13) 0.0504(13) -0.0125(10) -0.0038(11) -0.0066(10) Ag6 0.0478(11) 0.0709(13) 0.0429(12) -0.0008(10) 0.0012(10) 0.0156(9) P1 0.042(4) 0.039(4) 0.052(4) -0.004(3) -0.016(3) 0.001(3) P2 0.051(4) 0.048(4) 0.033(4) -0.003(3) -0.020(3) 0.010(3) P3 0.046(4) 0.041(4) 0.038(4) -0.002(3) -0.007(3) -0.003(3) P4 0.042(3) 0.045(4) 0.031(3) -0.004(3) -0.017(3) 0.004(3) O1 0.046(11) 0.097(16) 0.073(14) -0.036(11) -0.015(10) 0.016(10) O2 0.048(10) 0.059(11) 0.037(10) -0.009(8) -0.012(9) 0.008(8) O3 0.053(10) 0.056(11) 0.050(11) -0.011(8) 0.013(9) 0.013(8) O4 0.048(9) 0.055(11) 0.029(9) -0.004(8) -0.018(8) 0.002(8) N1 0.031(10) 0.049(12) 0.072(14) -0.004(10) -0.029(10) -0.004(9) N2 0.063(13) 0.041(11) 0.032(11) -0.003(8) -0.009(10) -0.007(9) N3 0.055(12) 0.041(11) 0.045(11) -0.007(9) 0.007(10) 0.023(9) N4 0.040(10) 0.053(12) 0.046(11) 0.017(10) -0.017(9) 0.001(9) N5 0.037(8) 0.060(8) 0.037(8) 0.002(7) -0.007(7) 0.017(7) N6 0.039(10) 0.072(13) 0.022(10) 0.001(9) -0.003(9) -0.020(9) N7 0.066(12) 0.029(10) 0.057(13) -0.007(9) -0.021(11) -0.001(9) N8 0.053(11) 0.032(10) 0.030(10) 0.014(8) -0.001(9) 0.002(9) N9 0.048(11) 0.076(13) 0.011(9) -0.007(9) -0.002(9) -0.005(10) N10 0.023(9) 0.063(12) 0.049(12) 0.006(10) -0.006(9) -0.004(8) N11 0.052(12) 0.063(12) 0.021(10) -0.009(9) -0.012(10) -0.006(10) N12 0.026(9) 0.059(13) 0.062(13) -0.005(11) -0.015(9) -0.001(9) C11 0.014(10) 0.061(13) 0.055(13) -0.010(12) 0.010(10) -0.010(10) N12A 0.030(9) 0.017(8) 0.064(12) -0.006(9) -0.005(9) 0.001(7) C13 0.049(13) 0.078(16) 0.038(13) -0.019(12) -0.014(11) 0.025(12) C14 0.055(13) 0.045(14) 0.039(13) 0.007(11) -0.019(12) 0.027(11) C15 0.041(13) 0.058(14) 0.055(15) -0.009(13) -0.016(12) 0.007(11) C16 0.043(12) 0.033(12) 0.053(14) 0.002(11) -0.006(11) 0.008(10) C21 0.040(12) 0.037(12) 0.051(14) 0.009(11) -0.019(11) -0.008(10) N22 0.075(14) 0.040(11) 0.074(15) -0.004(11) 0.020(12) -0.016(10) C23 0.074(17) 0.088(18) 0.13(2) -0.039(17) 0.035(17) -0.018(15) C24 0.100(13) 0.103(13) 0.113(13) -0.017(9) 0.006(9) -0.006(9) C25 0.071(18) 0.091(19) 0.13(2) -0.031(18) -0.044(18) -0.036(16) C26 0.064(16) 0.073(17) 0.079(18) -0.027(15) -0.026(15) 0.040(13) C31 0.050(12) 0.077(14) 0.010(10) -0.002(11) 0.006(10) -0.011(12) N32 0.034(7) 0.048(8) 0.025(7) 0.017(7) 0.006(6) -0.002(6) C33 0.051(15) 0.101(18) 0.070(17) 0.013(16) -0.003(14) -0.010(14) C34 0.066(17) 0.12(2) 0.094(19) 0.021(18) 0.030(16) 0.011(16) C35 0.045(14) 0.14(2) 0.050(15) 0.011(15) 0.033(13) 0.023(15) C36 0.051(14) 0.13(2) 0.020(12) -0.007(13) 0.005(12) 0.044(14) C41 0.020(10) 0.047(12) 0.047(13) -0.013(10) -0.021(10) 0.004(10) N42 0.067(13) 0.023(10) 0.069(13) -0.003(9) -0.011(11) 0.010(9) C43 0.036(13) 0.050(14) 0.116(19) -0.025(14) -0.015(14) -0.013(12) C44 0.077(17) 0.046(15) 0.12(2) -0.030(15) -0.026(17) -0.017(14) C45 0.081(17) 0.046(15) 0.095(18) -0.038(14) 0.023(15) -0.005(13) C46 0.040(12) 0.046(14) 0.047(13) -0.010(11) 0.017(11) -0.013(11) C51 0.033(11) 0.044(11) 0.023(11) 0.018(9) -0.002(10) 0.015(9) N52 0.020(9) 0.057(11) 0.038(11) 0.005(9) -0.002(8) -0.002(8) C53 0.024(11) 0.135(19) 0.053(15) -0.009(14) 0.010(12) 0.029(13) C54 0.063(16) 0.11(2) 0.060(16) 0.001(15) 0.007(15) 0.031(15) C55 0.076(17) 0.093(18) 0.032(14) -0.007(13) 0.019(14) 0.022(15) C56 0.056(14) 0.057(14) 0.039(14) 0.007(12) -0.009(13) 0.006(12) C61 0.044(12) 0.067(14) 0.025(11) -0.002(11) -0.009(11) -0.018(11) N62 0.054(11) 0.075(14) 0.042(11) 0.012(10) 0.010(10) -0.008(10) C63 0.060(14) 0.101(18) 0.043(14) 0.024(14) 0.015(13) -0.018(13) C64 0.071(16) 0.10(2) 0.024(13) 0.027(13) -0.005(13) -0.001(15) C65 0.073(16) 0.098(19) 0.049(15) -0.004(15) 0.012(14) 0.002(15) C66 0.050(13) 0.096(17) 0.028(13) 0.001(13) 0.005(12) -0.011(13) C71 0.027(10) 0.049(12) 0.022(11) -0.020(10) -0.015(9) 0.014(10) N72 0.066(12) 0.058(12) 0.025(10) -0.008(9) -0.008(10) -0.019(10) C73 0.086(17) 0.074(17) 0.062(16) -0.005(14) 0.006(15) -0.008(14) C74 0.069(15) 0.090(18) 0.080(17) 0.002(16) 0.029(15) 0.010(15) C75 0.083(16) 0.061(16) 0.043(14) 0.016(12) 0.005(13) -0.017(13) C76 0.069(14) 0.060(14) 0.029(12) -0.010(11) -0.016(12) -0.002(12) C81 0.041(12) 0.039(12) 0.035(11) -0.006(10) 0.006(10) 0.001(10) N82 0.038(11) 0.045(11) 0.073(13) -0.005(10) -0.019(10) 0.012(9) C83 0.033(13) 0.097(18) 0.087(18) -0.034(16) -0.022(13) 0.006(13) C84 0.027(12) 0.085(18) 0.101(19) -0.022(16) 0.003(13) -0.006(12) C85 0.068(15) 0.027(12) 0.081(16) -0.005(12) 0.029(13) -0.005(11) C86 0.072(15) 0.049(14) 0.049(13) 0.013(12) 0.009(13) 0.024(12) C91 0.029(11) 0.062(14) 0.030(12) 0.008(11) -0.004(10) -0.011(10) N92 0.047(11) 0.086(14) 0.020(10) 0.004(10) -0.006(9) 0.001(10) C93 0.055(10) 0.074(10) 0.049(10) -0.004(8) -0.003(8) 0.002(8) C94 0.024(12) 0.13(2) 0.068(17) -0.006(16) -0.005(13) 0.010(14) C95 0.037(13) 0.104(19) 0.069(17) -0.022(15) -0.003(14) 0.025(13) C96 0.050(13) 0.085(17) 0.052(15) -0.014(13) 0.032(13) 0.014(12) C101 0.028(11) 0.076(15) 0.057(14) -0.011(13) -0.010(11) 0.010(11) N102 0.052(12) 0.082(14) 0.048(12) 0.007(11) -0.004(10) 0.010(11) C103 0.045(13) 0.072(15) 0.079(16) 0.020(14) 0.044(13) 0.020(12) C104 0.056(14) 0.068(16) 0.047(14) 0.029(12) 0.021(12) 0.008(12) C105 0.055(15) 0.13(2) 0.066(17) 0.027(16) 0.028(14) 0.025(15) C106 0.045(13) 0.070(16) 0.068(16) -0.005(14) 0.011(13) 0.014(12) C111 0.063(14) 0.061(14) 0.044(14) -0.008(11) -0.023(13) -0.010(12) N112 0.043(11) 0.087(14) 0.045(12) -0.023(10) 0.020(10) -0.027(10) C113 0.093(18) 0.089(18) 0.099(19) -0.046(16) 0.025(16) -0.040(15) C114 0.084(11) 0.092(11) 0.087(11) -0.014(9) 0.020(9) -0.020(9) C115 0.070(16) 0.082(17) 0.076(16) -0.061(14) 0.031(14) -0.041(13) C116 0.061(15) 0.086(17) 0.032(13) -0.026(13) -0.005(12) -0.016(13) C121 0.055(13) 0.044(12) 0.044(13) 0.003(11) -0.003(11) -0.014(11) N122 0.039(10) 0.063(11) 0.029(10) -0.020(10) 0.002(9) 0.002(9) C123 0.066(15) 0.064(15) 0.052(14) 0.020(13) -0.038(13) 0.005(13) C124 0.059(15) 0.074(17) 0.067(17) 0.027(14) -0.016(14) -0.004(14) C125 0.083(16) 0.022(12) 0.067(16) 0.009(12) -0.009(15) -0.005(12) C126 0.032(8) 0.047(9) 0.042(9) -0.012(7) 0.014(7) 0.002(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 N12A 2.197(16) . ? Ag1 N42 2.203(17) . ? Ag2 N52 2.165(17) . ? Ag2 N32 2.187(16) . ? Ag3 N62 2.19(2) . ? Ag3 N22 2.19(2) . ? Ag4 N82 2.172(18) . ? Ag4 N122 2.185(18) . ? Ag5 N72 2.173(18) . ? Ag5 N112 2.177(19) . ? Ag6 N102 2.14(2) . ? Ag6 N92 2.192(19) . ? P1 O1 1.465(19) . ? P1 N1 1.649(18) . ? P1 N3 1.666(18) . ? P1 N2 1.68(2) . ? P2 O2 1.443(17) . ? P2 N6 1.653(19) . ? P2 N4 1.664(18) . ? P2 N5 1.668(19) . ? P3 O3 1.473(16) . ? P3 N7 1.595(19) . ? P3 N8 1.620(18) . ? P3 N9 1.684(17) . ? P4 O4 1.499(16) . ? P4 N11 1.627(18) . ? P4 N12 1.645(18) . ? P4 N10 1.682(19) . ? N1 C11 1.39(3) . ? N2 C21 1.44(3) . ? N3 C31 1.38(3) . ? N4 C41 1.37(3) . ? N5 C51 1.38(2) . ? N6 C61 1.36(3) . ? N7 C71 1.42(3) . ? N8 C81 1.41(3) . ? N9 C91 1.41(3) . ? N10 C101 1.49(3) . ? N11 C111 1.37(3) . ? N12 C121 1.43(3) . ? C11 N12A 1.31(3) . ? C11 C16 1.39(3) . ? N12A C13 1.37(3) . ? C13 C14 1.32(3) . ? C14 C15 1.38(3) . ? C15 C16 1.46(3) . ? C21 N22 1.27(3) . ? C21 C26 1.41(4) . ? N22 C23 1.31(3) . ? C23 C24 1.49(5) . ? C24 C25 1.29(5) . ? C25 C26 1.35(4) . ? C31 N32 1.31(3) . ? C31 C36 1.43(3) . ? N32 C33 1.27(3) . ? C33 C34 1.36(4) . ? C34 C35 1.32(4) . ? C35 C36 1.45(4) . ? C41 C46 1.35(3) . ? C41 N42 1.38(3) . ? N42 C43 1.32(3) . ? C43 C44 1.32(3) . ? C44 C45 1.48(4) . ? C45 C46 1.32(3) . ? C51 N52 1.40(3) . ? C51 C56 1.47(3) . ? N52 C53 1.36(3) . ? C53 C54 1.47(3) . ? C54 C55 1.39(4) . ? C55 C56 1.32(3) . ? C61 N62 1.35(3) . ? C61 C66 1.37(3) . ? N62 C63 1.40(3) . ? C63 C64 1.35(4) . ? C64 C65 1.38(4) . ? C65 C66 1.36(3) . ? C71 N72 1.31(3) . ? C71 C76 1.45(3) . ? N72 C73 1.37(3) . ? C73 C74 1.35(4) . ? C74 C75 1.35(4) . ? C75 C76 1.37(3) . ? C81 N82 1.31(3) . ? C81 C86 1.37(3) . ? N82 C83 1.45(3) . ? C83 C84 1.41(4) . ? C84 C85 1.37(3) . ? C85 C86 1.40(3) . ? C91 N92 1.29(3) . ? C91 C96 1.37(3) . ? N92 C93 1.36(3) . ? C93 C94 1.36(3) . ? C94 C95 1.32(4) . ? C95 C96 1.43(3) . ? C101 N102 1.34(3) . ? C101 C106 1.36(3) . ? N102 C103 1.34(3) . ? C103 C104 1.42(3) . ? C104 C105 1.41(3) . ? C105 C106 1.35(3) . ? C111 N112 1.36(3) . ? C111 C116 1.43(3) . ? N112 C113 1.33(3) . ? C113 C114 1.32(4) . ? C114 C115 1.41(4) . ? C115 C116 1.46(3) . ? C121 N122 1.36(3) . ? C121 C126 1.41(3) . ? N122 C123 1.34(3) . ? C123 C124 1.48(4) . ? C124 C125 1.32(4) . ? C125 C126 1.37(3) . ? N13 O6 1.205(13) . ? N13 O5 1.213(13) . ? N13 O7 1.221(13) . ? N14 O9 1.185(12) . ? N14 O8 1.196(12) . ? N14 O10 1.238(12) . ? N15 O12 1.190(12) . ? N15 O11 1.193(13) . ? N15 O13 1.257(12) . ? N16 O14 1.207(12) . ? N16 O15 1.210(12) . ? N16 O16 1.217(12) . ? N17 O17 1.178(12) . ? N17 O18 1.194(13) . ? N17 O19 1.233(12) . ? N18 O20 1.195(13) . ? N18 O21 1.208(12) . ? N18 O22 1.257(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 N12A Ag1 N42 171.6(7) . . ? N52 Ag2 N32 168.0(6) . . ? N62 Ag3 N22 172.6(8) . . ? N82 Ag4 N122 171.3(7) . . ? N72 Ag5 N112 177.4(8) . . ? N102 Ag6 N92 169.0(8) . . ? O1 P1 N1 116.3(10) . . ? O1 P1 N3 115.3(11) . . ? N1 P1 N3 103.8(10) . . ? O1 P1 N2 113.0(11) . . ? N1 P1 N2 100.9(10) . . ? N3 P1 N2 105.9(10) . . ? O2 P2 N6 116.3(10) . . ? O2 P2 N4 112.6(10) . . ? N6 P2 N4 102.4(10) . . ? O2 P2 N5 115.9(9) . . ? N6 P2 N5 104.7(10) . . ? N4 P2 N5 103.3(10) . . ? O3 P3 N7 115.6(10) . . ? O3 P3 N8 113.9(9) . . ? N7 P3 N8 104.9(10) . . ? O3 P3 N9 113.7(10) . . ? N7 P3 N9 103.3(10) . . ? N8 P3 N9 104.1(9) . . ? O4 P4 N11 117.7(10) . . ? O4 P4 N12 111.5(9) . . ? N11 P4 N12 107.3(9) . . ? O4 P4 N10 114.0(9) . . ? N11 P4 N10 101.0(9) . . ? N12 P4 N10 104.0(10) . . ? C11 N1 P1 127.6(17) . . ? C21 N2 P1 128.6(17) . . ? C31 N3 P1 130.0(16) . . ? C41 N4 P2 126.6(16) . . ? C51 N5 P2 123.9(15) . . ? C61 N6 P2 125.3(16) . . ? C71 N7 P3 127.6(16) . . ? C81 N8 P3 130.5(15) . . ? C91 N9 P3 127.4(15) . . ? C101 N10 P4 121.0(14) . . ? C111 N11 P4 128.4(17) . . ? C121 N12 P4 126.1(17) . . ? N12A C11 C16 124(2) . . ? N12A C11 N1 118(2) . . ? C16 C11 N1 118(2) . . ? C11 N12A C13 119.3(19) . . ? C11 N12A Ag1 123.6(15) . . ? C13 N12A Ag1 116.0(14) . . ? C14 C13 N12A 123(2) . . ? C13 C14 C15 120(2) . . ? C14 C15 C16 118(2) . . ? C11 C16 C15 115(2) . . ? N22 C21 C26 125(2) . . ? N22 C21 N2 116(2) . . ? C26 C21 N2 120(2) . . ? C21 N22 C23 120(2) . . ? C21 N22 Ag3 127.7(16) . . ? C23 N22 Ag3 112(2) . . ? N22 C23 C24 116(3) . . ? C25 C24 C23 125(4) . . ? C24 C25 C26 115(4) . . ? C25 C26 C21 119(3) . . ? N32 C31 N3 117.7(19) . . ? N32 C31 C36 125(2) . . ? N3 C31 C36 118(2) . . ? C33 N32 C31 115(2) . . ? C33 N32 Ag2 119.8(18) . . ? C31 N32 Ag2 124.5(14) . . ? N32 C33 C34 131(3) . . ? C35 C34 C33 113(3) . . ? C34 C35 C36 124(2) . . ? C31 C36 C35 112(2) . . ? C46 C41 N4 124.2(19) . . ? C46 C41 N42 118(2) . . ? N4 C41 N42 117.3(19) . . ? C43 N42 C41 121(2) . . ? C43 N42 Ag1 114.7(16) . . ? C41 N42 Ag1 123.8(15) . . ? N42 C43 C44 121(3) . . ? C43 C44 C45 119(3) . . ? C46 C45 C44 116(2) . . ? C45 C46 C41 123(2) . . ? N5 C51 N52 115.7(17) . . ? N5 C51 C56 124(2) . . ? N52 C51 C56 119.2(19) . . ? C53 N52 C51 120.0(18) . . ? C53 N52 Ag2 115.7(15) . . ? C51 N52 Ag2 124.1(13) . . ? N52 C53 C54 121(2) . . ? C55 C54 C53 117(3) . . ? C56 C55 C54 125(3) . . ? C55 C56 C51 118(2) . . ? N62 C61 N6 116(2) . . ? N62 C61 C66 120(2) . . ? N6 C61 C66 124(2) . . ? C61 N62 C63 120(2) . . ? C61 N62 Ag3 123.8(15) . . ? C63 N62 Ag3 114.4(18) . . ? C64 C63 N62 120(3) . . ? C63 C64 C65 118(2) . . ? C66 C65 C64 122(3) . . ? C65 C66 C61 119(3) . . ? N72 C71 N7 118.0(18) . . ? N72 C71 C76 123(2) . . ? N7 C71 C76 119(2) . . ? C71 N72 C73 116(2) . . ? C71 N72 Ag5 126.2(14) . . ? C73 N72 Ag5 116.1(17) . . ? C74 C73 N72 121(3) . . ? C73 C74 C75 125(3) . . ? C74 C75 C76 116(3) . . ? C75 C76 C71 119(2) . . ? N82 C81 C86 123(2) . . ? N82 C81 N8 115.7(19) . . ? C86 C81 N8 121(2) . . ? C81 N82 C83 118(2) . . ? C81 N82 Ag4 127.4(16) . . ? C83 N82 Ag4 112.4(16) . . ? C84 C83 N82 123(2) . . ? C85 C84 C83 112(2) . . ? C84 C85 C86 127(2) . . ? C81 C86 C85 116(2) . . ? N92 C91 C96 125(2) . . ? N92 C91 N9 114(2) . . ? C96 C91 N9 120(2) . . ? C91 N92 C93 115(2) . . ? C91 N92 Ag6 128.1(16) . . ? C93 N92 Ag6 116.6(16) . . ? C94 C93 N92 124(2) . . ? C95 C94 C93 119(3) . . ? C94 C95 C96 118(2) . . ? C91 C96 C95 117(2) . . ? N102 C101 C106 127(3) . . ? N102 C101 N10 108.9(19) . . ? C106 C101 N10 124(2) . . ? C101 N102 C103 113(2) . . ? C101 N102 Ag6 130.5(17) . . ? C103 N102 Ag6 116.2(17) . . ? N102 C103 C104 126(2) . . ? C105 C104 C103 116(2) . . ? C106 C105 C104 119(2) . . ? C105 C106 C101 119(3) . . ? N112 C111 N11 119(2) . . ? N112 C111 C116 122(2) . . ? N11 C111 C116 119(2) . . ? C113 N112 C111 120(2) . . ? C113 N112 Ag5 115.9(17) . . ? C111 N112 Ag5 124.2(15) . . ? C114 C113 N112 125(3) . . ? C113 C114 C115 118(3) . . ? C114 C115 C116 121(2) . . ? C111 C116 C115 114(2) . . ? N122 C121 C126 124(2) . . ? N122 C121 N12 116(2) . . ? C126 C121 N12 120(2) . . ? C123 N122 C121 115(2) . . ? C123 N122 Ag4 119.0(16) . . ? C121 N122 Ag4 125.6(15) . . ? N122 C123 C124 125(2) . . ? C125 C124 C123 114(2) . . ? C124 C125 C126 125(3) . . ? C125 C126 C121 117(2) . . ? O6 N13 O5 117.3(19) . . ? O6 N13 O7 118.7(19) . . ? O5 N13 O7 112.8(17) . . ? O9 N14 O8 123.0(16) . . ? O9 N14 O10 119.5(15) . . ? O8 N14 O10 115.5(15) . . ? O12 N15 O11 124.0(17) . . ? O12 N15 O13 117.9(16) . . ? O11 N15 O13 117.8(16) . . ? O14 N16 O15 113.3(16) . . ? O14 N16 O16 123.7(16) . . ? O15 N16 O16 122.0(16) . . ? O17 N17 O18 127.4(17) . . ? O17 N17 O19 119.0(15) . . ? O18 N17 O19 113.7(16) . . ? O20 N18 O21 125.3(17) . . ? O20 N18 O22 117.8(16) . . ? O21 N18 O22 116.6(15) . . ? 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 N1 H1 O10 0.86 2.37 3.09(3) 141.5 . N1 H1 O9 0.86 2.63 3.47(3) 166.7 . N2 H2 O13 0.86 2.25 3.05(2) 155.9 . N3 H3 O5 0.86 2.38 3.21(2) 162.7 . N4 H4 O13 0.86 2.34 3.14(2) 155.0 . N5 H5 O10 0.86 2.37 3.10(2) 142.7 . N5 H5 O8 0.86 2.42 3.24(3) 161.1 . N6 H6 O7 0.86 2.23 3.00(3) 147.7 . N7 H7 O19 0.86 2.29 3.05(3) 146.4 . N8 H8 O22 0.86 2.36 3.15(2) 153.9 . N9 H9 O16 0.86 2.48 3.24(2) 148.5 . N9 H9 O15 0.86 2.54 3.34(3) 154.9 . N10 H10 O17 0.86 2.18 3.01(2) 161.5 . N10 H10 O19 0.86 2.37 3.11(2) 144.1 . N11 H11 O22 0.86 2.24 3.05(2) 156.1 . N12 H12 O16 0.86 2.30 3.03(3) 143.7 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 22.51 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.911 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.188 # Attachment '- compound3a_new.cif' data_compound3a _database_code_depnum_ccdc_archive 'CCDC 865264' #TrackingRef '- compound3a_new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H54 Ag8 N24 O4 P4 4+, (Cl O4 1-)4, (C H4 O)5, (H2 O)3' _chemical_formula_sum 'C65 H80 Ag8 Cl4 N24 O28 P4' _chemical_formula_weight 2774.17 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.075(3) _cell_length_b 13.2864(7) _cell_length_c 27.6363(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.737(2) _cell_angle_gamma 90.00 _cell_volume 18018.2(17) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 147 _cell_measurement_theta_min 4.10 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 2.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10928 _exptl_absorpt_coefficient_mu 1.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6356 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Apex II' _diffrn_measurement_method 'Omega and phi scans' _diffrn_reflns_number 104049 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 25.03 _reflns_number_total 15837 _reflns_number_gt 8982 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. All perchlorate ions and solvents molecules are disordered. Perchlorate ions were split over several positions and refined with restraints (SAME and SIMU). The disorder of solvent molecules could not be resolved. Large peaks of residual electron density were refined as partially occupied O-atoms. ; _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^)+(0.1196P)^2^+105.6329P] 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_number_reflns 15837 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 1195 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.2278 _refine_ls_wR_factor_gt 0.1861 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 0.998 _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 0.127706(14) 0.36073(6) -0.01805(3) 0.0613(2) Uani 1 1 d . . . Ag2 Ag 0.110050(17) 0.40462(6) 0.07975(3) 0.0647(2) Uani 1 1 d . . . Ag3 Ag 0.103427(19) 0.47897(7) 0.17235(3) 0.0798(3) Uani 1 1 d . . . Ag4 Ag 0.137021(19) 0.67290(7) 0.11899(3) 0.0787(3) Uani 1 1 d . . . Ag5 Ag 0.14726(2) 0.29574(8) -0.10566(3) 0.0893(3) Uani 1 1 d . . . Ag6 Ag 0.07945(2) 0.41998(8) -0.11815(3) 0.0965(3) Uani 1 1 d . . . Ag7 Ag 0.19238(2) 0.20994(8) -0.01762(4) 0.0958(4) Uani 1 1 d . . . Ag8 Ag 0.06962(2) 0.23755(9) 0.14510(3) 0.1007(4) Uani 1 1 d . . . P1 P 0.06318(5) 0.3086(2) -0.02528(9) 0.0570(6) Uani 1 1 d . . . P2 P 0.12227(5) 0.1694(2) 0.09770(9) 0.0587(6) Uani 1 1 d . . . P3 P 0.18513(5) 0.41489(19) 0.03175(9) 0.0558(6) Uani 1 1 d . . . P4 P 0.10493(5) 0.61781(19) 0.02421(9) 0.0567(6) Uani 1 1 d . . . O1 O 0.05969(12) 0.4176(5) -0.0333(2) 0.0638(17) Uani 1 1 d . . . O2 O 0.09569(13) 0.1566(5) 0.0744(2) 0.0670(18) Uani 1 1 d . . . O3 O 0.18181(12) 0.3162(5) 0.0550(2) 0.0623(16) Uani 1 1 d . . . O4 O 0.13484(13) 0.6265(5) 0.0293(2) 0.0620(16) Uani 1 1 d . . . N1 N 0.05547(16) 0.2786(6) 0.0308(3) 0.064(2) Uani 1 1 d . . . H1A H 0.0655 0.2336 0.0447 0.077 Uiso 1 1 calc R . . N2 N 0.04097(15) 0.2420(6) -0.0587(3) 0.063(2) Uani 1 1 d . . . H2 H 0.0285 0.2113 -0.0427 0.076 Uiso 1 1 calc R . . N3 N 0.09368(15) 0.2703(6) -0.0356(3) 0.0569(19) Uani 1 1 d . . . N4 N 0.12806(17) 0.0857(6) 0.1428(3) 0.066(2) Uani 1 1 d . . . H4A H 0.1401 0.0400 0.1375 0.080 Uiso 1 1 calc R . . N5 N 0.14769(16) 0.1465(6) 0.0602(3) 0.063(2) Uani 1 1 d . . . H5 H 0.1594 0.1942 0.0572 0.076 Uiso 1 1 calc R . . N6 N 0.12690(15) 0.2822(6) 0.1182(3) 0.0571(19) Uani 1 1 d . . . N7 N 0.17690(16) 0.5080(6) 0.0690(3) 0.067(2) Uani 1 1 d . . . H7 H 0.1649 0.5501 0.0585 0.080 Uiso 1 1 calc R . . N8 N 0.21803(15) 0.4376(6) 0.0192(3) 0.066(2) Uani 1 1 d . . . H8A H 0.2264 0.4807 0.0373 0.079 Uiso 1 1 calc R . . N9 N 0.16690(15) 0.4290(6) -0.0164(3) 0.0582(19) Uani 1 1 d . . . N10 N 0.09702(16) 0.5780(6) -0.0313(3) 0.065(2) Uani 1 1 d . . . H10 H 0.0848 0.5317 -0.0338 0.078 Uiso 1 1 calc R . . N11 N 0.09033(16) 0.7309(6) 0.0274(3) 0.062(2) Uani 1 1 d . . . H11 H 0.0844 0.7557 0.0005 0.075 Uiso 1 1 calc R . . N12 N 0.09074(16) 0.5428(6) 0.0618(3) 0.061(2) Uani 1 1 d . . . N16 N 0.03641(17) 0.3114(7) 0.1062(3) 0.075(3) Uani 1 1 d . . . N26 N 0.05213(18) 0.2917(7) -0.1365(3) 0.078(2) Uani 1 1 d . . . N36 N 0.12046(17) 0.1712(7) -0.0867(3) 0.067(2) Uani 1 1 d . B . N46 N 0.09304(19) 0.1398(7) 0.1947(3) 0.075(2) Uani 1 1 d . . . N56 N 0.17074(17) 0.0711(6) -0.0025(3) 0.067(2) Uani 1 1 d . . . N66 N 0.13843(18) 0.3826(7) 0.1852(3) 0.072(2) Uani 1 1 d . . . N76 N 0.17501(18) 0.6007(7) 0.1397(3) 0.074(2) Uani 1 1 d . . . N86 N 0.22527(18) 0.3098(8) -0.0384(3) 0.076(2) Uani 1 1 d . . . N96 N 0.17207(18) 0.4310(8) -0.1001(3) 0.080(3) Uani 1 1 d . B . N106 N 0.1028(2) 0.5572(7) -0.1135(3) 0.089(3) Uani 1 1 d . . . N116 N 0.10054(17) 0.7691(6) 0.1080(3) 0.070(2) Uani 1 1 d . . . N126 N 0.06905(19) 0.5562(7) 0.1374(3) 0.075(2) Uani 1 1 d . . . C11 C 0.0340(2) 0.3195(8) 0.0584(4) 0.062(3) Uani 1 1 d . . . C12 C 0.0123(2) 0.3678(9) 0.0347(4) 0.077(3) Uani 1 1 d . . . H12 H 0.0112 0.3723 0.0012 0.092 Uiso 1 1 calc R . . C13 C -0.0074(2) 0.4084(10) 0.0643(5) 0.087(4) Uani 1 1 d . . . H13 H -0.0222 0.4417 0.0503 0.104 Uiso 1 1 calc R . . C14 C -0.0055(2) 0.4008(11) 0.1143(5) 0.098(4) Uani 1 1 d . . . H14 H -0.0186 0.4286 0.1344 0.118 Uiso 1 1 calc R . . C15 C 0.0168(3) 0.3497(11) 0.1324(4) 0.099(4) Uani 1 1 d . . . H15 H 0.0180 0.3417 0.1657 0.119 Uiso 1 1 calc R . . C21 C 0.0398(2) 0.2291(8) -0.1087(4) 0.066(3) Uani 1 1 d . . . C22 C 0.0244(3) 0.1473(11) -0.1268(5) 0.102(4) Uani 1 1 d . . . H22 H 0.0159 0.1024 -0.1060 0.122 Uiso 1 1 calc R . . C23 C 0.0224(4) 0.1361(15) -0.1772(7) 0.131(6) Uani 1 1 d . . . H23 H 0.0125 0.0824 -0.1900 0.157 Uiso 1 1 calc R . . C24 C 0.0344(3) 0.2009(13) -0.2074(5) 0.111(5) Uani 1 1 d . . . H24 H 0.0325 0.1961 -0.2408 0.134 Uiso 1 1 calc R . . C25 C 0.0498(3) 0.2754(11) -0.1853(5) 0.103(4) Uani 1 1 d . . . H25 H 0.0594 0.3184 -0.2054 0.124 Uiso 1 1 calc R . . C31 C 0.1000(2) 0.1745(7) -0.0549(3) 0.057(2) Uani 1 1 d . B . C32 C 0.0857(2) 0.0889(9) -0.0412(4) 0.077(3) Uani 1 1 d . . . H32 H 0.0719 0.0922 -0.0184 0.093 Uiso 1 1 calc R B . C33 C 0.0928(3) -0.0015(10) -0.0628(6) 0.100(4) Uani 1 1 d . . . H33 H 0.0840 -0.0607 -0.0541 0.121 Uiso 1 1 calc R . . C34 C 0.1124(3) -0.0029(11) -0.0964(5) 0.106(5) Uani 1 1 d . . . H34 H 0.1165 -0.0621 -0.1128 0.127 Uiso 1 1 calc R B . C35 C 0.1261(3) 0.0837(11) -0.1060(5) 0.091(4) Uani 1 1 d . B . H35 H 0.1404 0.0806 -0.1277 0.109 Uiso 1 1 calc R . . C41 C 0.1155(2) 0.0829(8) 0.1874(4) 0.068(3) Uani 1 1 d . . . C42 C 0.1263(3) 0.0171(11) 0.2214(4) 0.100(4) Uani 1 1 d . . . H42 H 0.1416 -0.0220 0.2152 0.120 Uiso 1 1 calc R . . C43 C 0.1128(4) 0.0130(14) 0.2657(5) 0.125(6) Uani 1 1 d . . . H43 H 0.1193 -0.0309 0.2894 0.150 Uiso 1 1 calc R . . C44 C 0.0910(4) 0.0692(13) 0.2755(5) 0.138(7) Uani 1 1 d . . . H44 H 0.0824 0.0669 0.3053 0.166 Uiso 1 1 calc R . . C45 C 0.0824(3) 0.1284(11) 0.2400(5) 0.107(5) Uani 1 1 d . . . H45 H 0.0671 0.1673 0.2465 0.128 Uiso 1 1 calc R . . C51 C 0.1526(2) 0.0596(8) 0.0325(4) 0.064(3) Uani 1 1 d . . . C52 C 0.1405(2) -0.0310(8) 0.0414(4) 0.074(3) Uani 1 1 d . . . H52 H 0.1270 -0.0362 0.0647 0.089 Uiso 1 1 calc R . . C53 C 0.1482(3) -0.1129(10) 0.0163(5) 0.089(4) Uani 1 1 d . . . H53 H 0.1401 -0.1749 0.0222 0.107 Uiso 1 1 calc R . . C54 C 0.1682(2) -0.1051(9) -0.0183(5) 0.087(4) Uani 1 1 d . . . H54 H 0.1746 -0.1614 -0.0346 0.104 Uiso 1 1 calc R . . C55 C 0.1780(2) -0.0125(9) -0.0275(4) 0.083(3) Uani 1 1 d . . . H55 H 0.1905 -0.0053 -0.0524 0.100 Uiso 1 1 calc R . . C61 C 0.1445(2) 0.3018(8) 0.1567(4) 0.061(3) Uani 1 1 d . . . C62 C 0.1680(2) 0.2476(9) 0.1675(4) 0.073(3) Uani 1 1 d . . . H62 H 0.1735 0.1965 0.1468 0.087 Uiso 1 1 calc R . . C63 C 0.1831(2) 0.2684(11) 0.2083(4) 0.090(4) Uani 1 1 d . . . H63 H 0.1979 0.2280 0.2166 0.108 Uiso 1 1 calc R . . C64 C 0.1766(3) 0.3472(12) 0.2367(4) 0.098(4) Uani 1 1 d . . . H64 H 0.1869 0.3628 0.2641 0.118 Uiso 1 1 calc R . . C65 C 0.1545(3) 0.4031(11) 0.2238(4) 0.089(4) Uani 1 1 d . . . H65 H 0.1502 0.4586 0.2427 0.106 Uiso 1 1 calc R . . C71 C 0.1874(2) 0.5251(8) 0.1156(4) 0.067(3) Uani 1 1 d . . . C72 C 0.2091(2) 0.4751(10) 0.1344(4) 0.083(3) Uani 1 1 d . . . H72 H 0.2168 0.4230 0.1169 0.100 Uiso 1 1 calc R . . C73 C 0.2196(3) 0.4992(12) 0.1781(5) 0.099(4) Uani 1 1 d . . . H73 H 0.2341 0.4632 0.1915 0.119 Uiso 1 1 calc R . . C74 C 0.2078(3) 0.5815(12) 0.2028(5) 0.097(4) Uani 1 1 d . . . H74 H 0.2152 0.6034 0.2322 0.116 Uiso 1 1 calc R . . C75 C 0.1859(3) 0.6274(10) 0.1835(4) 0.088(4) Uani 1 1 d . . . H75 H 0.1778 0.6795 0.2006 0.105 Uiso 1 1 calc R . . C81 C 0.23294(19) 0.3943(9) -0.0170(4) 0.069(3) Uani 1 1 d . . . C82 C 0.2564(2) 0.4493(11) -0.0321(5) 0.093(4) Uani 1 1 d . . . H82 H 0.2609 0.5110 -0.0182 0.112 Uiso 1 1 calc R . . C83 C 0.2723(3) 0.4086(16) -0.0679(6) 0.115(5) Uani 1 1 d . . . H83 H 0.2885 0.4393 -0.0768 0.138 Uiso 1 1 calc R . . C84 C 0.2637(3) 0.3214(16) -0.0901(6) 0.114(6) Uani 1 1 d . . . H84 H 0.2732 0.2956 -0.1162 0.137 Uiso 1 1 calc R . . C85 C 0.2415(3) 0.2736(10) -0.0740(4) 0.089(4) Uani 1 1 d . . . H85 H 0.2369 0.2122 -0.0880 0.107 Uiso 1 1 calc R . . C91 C 0.17654(19) 0.4775(8) -0.0571(4) 0.067(3) Uani 1 1 d . B . C92 C 0.1900(2) 0.5707(9) -0.0546(5) 0.084(3) Uani 1 1 d . . . H92 H 0.1905 0.6064 -0.0257 0.101 Uiso 1 1 calc R B . C93 C 0.2021(3) 0.6085(12) -0.0941(7) 0.113(5) Uani 1 1 d . . . H93 H 0.2124 0.6672 -0.0921 0.136 Uiso 1 1 calc R . . C94 C 0.1992(3) 0.5619(16) -0.1351(7) 0.139(7) Uani 1 1 d . . . H94 H 0.2071 0.5887 -0.1626 0.167 Uiso 1 1 calc R B . C95 C 0.1846(3) 0.4737(14) -0.1388(5) 0.117(5) Uani 1 1 d . B . H95 H 0.1833 0.4420 -0.1688 0.140 Uiso 1 1 calc R . . C101 C 0.1083(2) 0.6128(8) -0.0738(4) 0.066(3) Uani 1 1 d . . . C102 C 0.1246(3) 0.6967(9) -0.0754(4) 0.084(3) Uani 1 1 d . . . H102 H 0.1283 0.7330 -0.0473 0.101 Uiso 1 1 calc R . . C103 C 0.1356(3) 0.7275(9) -0.1196(5) 0.094(4) Uani 1 1 d . . . H103 H 0.1471 0.7831 -0.1212 0.112 Uiso 1 1 calc R . . C104 C 0.1292(4) 0.6751(11) -0.1593(5) 0.149(8) Uani 1 1 d . . . H104 H 0.1357 0.6956 -0.1892 0.179 Uiso 1 1 calc R . . C105 C 0.1126(4) 0.5889(11) -0.1561(4) 0.123(6) Uani 1 1 d . . . H105 H 0.1084 0.5531 -0.1841 0.148 Uiso 1 1 calc R . . C111 C 0.0865(2) 0.7894(8) 0.0679(4) 0.070(3) Uani 1 1 d . . . C112 C 0.0670(2) 0.8698(9) 0.0678(5) 0.089(4) Uani 1 1 d . . . H112 H 0.0578 0.8848 0.0391 0.107 Uiso 1 1 calc R . . C113 C 0.0616(3) 0.9233(10) 0.1066(6) 0.093(4) Uani 1 1 d . . . H113 H 0.0494 0.9768 0.1053 0.112 Uiso 1 1 calc R . . C114 C 0.0748(3) 0.8967(10) 0.1494(6) 0.106(5) Uani 1 1 d . . . H114 H 0.0700 0.9279 0.1781 0.127 Uiso 1 1 calc R . . C115 C 0.0948(3) 0.8256(8) 0.1497(4) 0.081(3) Uani 1 1 d . . . H115 H 0.1048 0.8142 0.1779 0.097 Uiso 1 1 calc R . . C121 C 0.0676(2) 0.5688(7) 0.0892(4) 0.062(3) Uani 1 1 d . . . C122 C 0.0447(2) 0.6078(10) 0.0686(5) 0.083(3) Uani 1 1 d . . . H122 H 0.0432 0.6118 0.0351 0.100 Uiso 1 1 calc R . . C123 C 0.0242(3) 0.6407(12) 0.0961(6) 0.106(4) Uani 1 1 d . . . H123 H 0.0087 0.6695 0.0820 0.127 Uiso 1 1 calc R . . C124 C 0.0265(3) 0.6307(12) 0.1451(6) 0.115(5) Uani 1 1 d . . . H124 H 0.0128 0.6548 0.1650 0.138 Uiso 1 1 calc R . . C125 C 0.0482(3) 0.5866(11) 0.1642(5) 0.100(4) Uani 1 1 d . . . H125 H 0.0491 0.5765 0.1975 0.120 Uiso 1 1 calc R . . Cl1 Cl 0.12691(19) 0.3049(7) -0.2294(3) 0.0912(19) Uiso 0.33 1 d PDU A 1 O11 O 0.1227(4) 0.3881(11) -0.1967(6) 0.112(4) Uiso 0.33 1 d PDU A 1 O12 O 0.1213(4) 0.3365(15) -0.2785(4) 0.102(4) Uiso 0.33 1 d PDU A 1 O13 O 0.1549(2) 0.2717(15) -0.2251(8) 0.123(5) Uiso 0.33 1 d PDU A 1 O14 O 0.1088(4) 0.2232(11) -0.2173(7) 0.107(4) Uiso 0.33 1 d PDU A 1 Cl1' Cl 0.11429(18) 0.3425(7) -0.2316(3) 0.099(2) Uiso 0.33 1 d PDU B 2 O11' O 0.1256(4) 0.3433(15) -0.1831(4) 0.100(3) Uiso 0.33 1 d PDU B 2 O12' O 0.0927(3) 0.4158(12) -0.2355(7) 0.132(4) Uiso 0.33 1 d PDU B 2 O13' O 0.1036(4) 0.2433(9) -0.2420(7) 0.116(4) Uiso 0.33 1 d PDU B 2 O14' O 0.1352(3) 0.3674(15) -0.2658(6) 0.114(4) Uiso 0.33 1 d PDU B 2 Cl1" Cl 0.12673(19) 0.3139(7) -0.2292(3) 0.0910(19) Uiso 0.33 1 d PDU C 3 O11" O 0.1107(3) 0.3713(13) -0.2637(6) 0.111(4) Uiso 0.33 1 d PDU C 3 O12" O 0.1384(4) 0.2273(11) -0.2528(7) 0.108(5) Uiso 0.33 1 d PDU C 3 O13" O 0.1482(3) 0.3770(13) -0.2100(7) 0.105(4) Uiso 0.33 1 d PDU C 3 O14" O 0.1096(4) 0.2800(15) -0.1904(6) 0.105(4) Uiso 0.33 1 d PDU C 3 Cl2 Cl 0.31350(17) 0.4005(6) 0.3506(3) 0.223(4) Uiso 0.75 1 d PDU . . O21 O 0.3188(3) 0.5064(7) 0.3578(5) 0.150(5) Uiso 0.75 1 d PDU . . O22 O 0.3389(3) 0.3462(11) 0.3482(8) 0.270(8) Uiso 0.75 1 d PDU . . O23 O 0.2976(4) 0.3633(13) 0.3904(6) 0.278(8) Uiso 0.75 1 d PDU . . O24 O 0.2986(4) 0.3862(13) 0.3057(5) 0.293(9) Uiso 0.75 1 d PDU . . Cl3 Cl 0.20280(13) 0.0749(5) 0.3399(2) 0.170(3) Uiso 0.75 1 d PDU . . O31 O 0.2107(3) -0.0213(8) 0.3600(5) 0.209(7) Uiso 0.75 1 d PDU . . O32 O 0.2133(3) 0.0845(13) 0.2916(4) 0.229(7) Uiso 0.75 1 d PDU . . O33 O 0.17343(16) 0.0813(13) 0.3384(6) 0.219(7) Uiso 0.75 1 d PDU . . O34 O 0.2138(3) 0.1550(9) 0.3696(5) 0.231(7) Uiso 0.75 1 d PDU . . Cl4 Cl 0.0530(2) 0.6165(8) -0.2260(3) 0.179(3) Uiso 0.505(9) 1 d PDU D 1 O41 O 0.0610(4) 0.6864(14) -0.1883(6) 0.198(7) Uiso 0.505(9) 1 d PDU D 1 O42 O 0.0725(3) 0.6204(16) -0.2647(6) 0.173(6) Uiso 0.505(9) 1 d PDU D 1 O43 O 0.0263(3) 0.6436(16) -0.2442(7) 0.177(5) Uiso 0.505(9) 1 d PDU D 1 O44 O 0.0524(4) 0.5155(10) -0.2066(7) 0.178(5) Uiso 0.505(9) 1 d PDU D 1 Cl4' Cl 0.0527(2) 0.5758(8) -0.2345(3) 0.171(3) Uiso 0.495(9) 1 d PDU B 2 O41' O 0.0559(5) 0.6293(14) -0.1893(5) 0.197(5) Uiso 0.495(9) 1 d PDU B 2 O42' O 0.0266(3) 0.5257(14) -0.2360(7) 0.169(6) Uiso 0.495(9) 1 d PDU B 2 O43' O 0.0742(3) 0.5024(12) -0.2384(7) 0.158(4) Uiso 0.495(9) 1 d PDU B 2 O44' O 0.0540(4) 0.6459(12) -0.2744(6) 0.177(5) Uiso 0.495(9) 1 d PDU B 2 Cl5 Cl -0.00112(15) 1.0249(6) 0.4889(3) 0.130(3) Uiso 0.50 1 d PDU E -1 O51 O -0.0245(3) 0.9805(15) 0.5119(7) 0.187(8) Uiso 0.50 1 d PDU E -1 O52 O 0.0054(4) 1.1199(9) 0.5116(6) 0.143(6) Uiso 0.50 1 d PDU E -1 O53 O -0.0074(4) 1.0409(15) 0.4383(4) 0.197(8) Uiso 0.50 1 d PDU E -1 O54 O 0.0220(3) 0.9583(14) 0.4937(7) 0.175(8) Uiso 0.50 1 d PDU E -1 O1S O 0.2664(7) 0.237(3) 0.4501(12) 0.204(13) Uiso 0.50 1 d P . . O2S O 0.2499(6) 0.106(2) 0.4477(9) 0.136(8) Uiso 0.50 1 d P . . O3S O 0.2624(9) 0.148(4) 0.4427(16) 0.232(18) Uiso 0.50 1 d P . . O4S O 0.0482(3) 0.2099(12) 0.4587(6) 0.080(5) Uiso 0.50 1 d P . . O5S O 0.0561(4) 0.2336(17) 0.4370(8) 0.116(7) Uiso 0.50 1 d P . . O6S O 0.0513(6) 0.190(2) 0.3626(11) 0.185(11) Uiso 0.50 1 d P . . O7S O 0.2461(5) 0.3043(17) 0.2879(8) 0.135(7) Uiso 0.50 1 d P . . O8S O 0.2653(6) 0.543(2) 0.2948(11) 0.191(11) Uiso 0.50 1 d P . . O9S O 0.2611(6) 0.242(2) 0.2021(11) 0.187(11) Uiso 0.50 1 d P . . O10S O 0.1853(5) 1.200(2) 0.8464(9) 0.145(8) Uiso 0.50 1 d P . . O11S O 0.1975(7) 1.141(3) 0.8263(12) 0.189(11) Uiso 0.50 1 d P . . O12S O -0.0060(6) -0.1231(19) -0.2342(10) 0.169(10) Uiso 0.50 1 d P . . 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 0.0496(4) 0.0736(5) 0.0608(5) -0.0066(4) 0.0041(3) -0.0069(4) Ag2 0.0832(6) 0.0590(5) 0.0519(4) 0.0048(3) 0.0039(4) 0.0051(4) Ag3 0.1003(7) 0.0846(6) 0.0546(5) -0.0004(4) 0.0046(4) 0.0136(5) Ag4 0.0871(6) 0.0819(6) 0.0668(5) -0.0092(4) -0.0095(4) 0.0199(5) Ag5 0.0925(7) 0.1133(8) 0.0625(5) -0.0139(5) 0.0143(5) -0.0197(6) Ag6 0.1336(9) 0.0904(7) 0.0656(6) -0.0094(5) 0.0126(5) -0.0361(6) Ag7 0.1087(8) 0.0830(7) 0.0966(7) -0.0202(5) 0.0406(6) -0.0295(5) Ag8 0.0942(7) 0.1389(9) 0.0693(6) 0.0251(6) 0.0121(5) 0.0404(6) P1 0.0471(14) 0.0673(17) 0.0564(15) 0.0027(12) -0.0011(11) -0.0036(12) P2 0.0601(16) 0.0576(16) 0.0586(15) 0.0075(12) 0.0048(12) -0.0037(12) P3 0.0474(14) 0.0580(16) 0.0621(15) -0.0026(12) 0.0037(11) -0.0037(11) P4 0.0630(16) 0.0559(15) 0.0509(14) 0.0009(11) -0.0048(12) 0.0035(12) O1 0.054(4) 0.075(5) 0.062(4) 0.005(3) -0.003(3) -0.006(3) O2 0.063(4) 0.066(4) 0.072(4) 0.004(3) 0.001(3) -0.002(3) O3 0.057(4) 0.059(4) 0.072(4) 0.004(3) 0.011(3) -0.005(3) O4 0.067(4) 0.064(4) 0.055(4) -0.010(3) -0.004(3) 0.002(3) N1 0.058(5) 0.073(6) 0.062(5) 0.007(4) 0.002(4) 0.006(4) N2 0.048(4) 0.085(6) 0.058(5) -0.002(4) -0.002(4) -0.010(4) N3 0.050(4) 0.061(5) 0.060(5) -0.003(4) -0.001(4) -0.007(4) N4 0.071(5) 0.066(5) 0.063(5) 0.010(4) 0.010(4) 0.011(4) N5 0.064(5) 0.057(5) 0.070(5) 0.001(4) 0.013(4) -0.004(4) N6 0.058(5) 0.058(5) 0.056(5) 0.005(4) 0.004(4) -0.002(4) N7 0.064(5) 0.075(6) 0.062(5) -0.009(4) -0.012(4) 0.006(4) N8 0.045(4) 0.083(6) 0.068(5) -0.003(4) 0.000(4) -0.013(4) N9 0.055(5) 0.061(5) 0.059(5) -0.003(4) 0.001(4) -0.005(4) N10 0.062(5) 0.071(6) 0.061(5) 0.004(4) 0.003(4) -0.015(4) N11 0.064(5) 0.066(5) 0.056(5) 0.003(4) -0.001(4) 0.011(4) N12 0.074(5) 0.058(5) 0.052(5) -0.001(4) 0.001(4) 0.008(4) N16 0.059(5) 0.105(7) 0.062(6) 0.014(5) 0.023(4) 0.016(5) N26 0.072(6) 0.091(7) 0.071(6) 0.001(5) 0.004(5) -0.013(5) N36 0.065(5) 0.077(6) 0.059(5) -0.012(4) 0.008(4) 0.004(4) N46 0.087(6) 0.088(7) 0.051(5) 0.007(4) 0.009(4) 0.010(5) N56 0.062(5) 0.063(6) 0.076(6) -0.006(4) 0.000(4) -0.008(4) N66 0.088(6) 0.076(6) 0.052(5) 0.010(4) 0.007(5) -0.001(5) N76 0.080(6) 0.085(6) 0.056(5) -0.001(5) 0.005(4) -0.003(5) N86 0.065(6) 0.080(7) 0.084(7) 0.014(5) 0.012(5) 0.000(5) N96 0.077(6) 0.107(8) 0.056(6) 0.016(5) 0.000(5) -0.004(5) N106 0.132(9) 0.067(6) 0.069(6) -0.003(5) 0.010(6) -0.016(6) N116 0.071(6) 0.070(6) 0.068(6) -0.001(5) -0.004(5) 0.007(4) N126 0.092(7) 0.082(6) 0.052(5) 0.001(4) 0.009(5) 0.009(5) C11 0.061(6) 0.065(6) 0.061(6) 0.005(5) 0.018(5) -0.006(5) C12 0.045(6) 0.100(9) 0.084(8) 0.012(7) 0.004(5) 0.002(6) C13 0.046(6) 0.127(11) 0.087(9) 0.008(7) 0.002(6) 0.013(6) C14 0.061(7) 0.141(12) 0.093(10) -0.009(8) 0.013(7) 0.022(7) C15 0.093(9) 0.142(12) 0.062(7) 0.022(7) 0.014(7) 0.016(9) C21 0.050(6) 0.077(7) 0.072(7) -0.008(6) -0.013(5) -0.001(5) C22 0.112(11) 0.106(11) 0.086(9) 0.005(8) -0.015(8) -0.019(8) C23 0.136(14) 0.142(15) 0.113(13) -0.038(11) -0.024(11) -0.033(12) C24 0.135(13) 0.124(13) 0.074(9) -0.028(9) -0.010(9) -0.015(10) C25 0.118(11) 0.118(11) 0.075(9) 0.001(8) 0.017(8) -0.026(9) C31 0.060(6) 0.054(6) 0.057(6) -0.002(5) -0.014(5) -0.008(5) C32 0.080(8) 0.069(8) 0.084(8) 0.005(6) -0.004(6) 0.000(6) C33 0.124(12) 0.062(9) 0.115(11) 0.006(7) -0.023(9) -0.015(8) C34 0.139(13) 0.079(10) 0.100(11) -0.024(8) 0.002(10) 0.031(9) C35 0.098(9) 0.093(10) 0.082(8) -0.028(8) 0.000(7) 0.016(8) C41 0.087(8) 0.068(7) 0.049(6) 0.002(5) 0.000(5) 0.005(6) C42 0.116(10) 0.119(11) 0.064(8) 0.015(7) -0.008(7) 0.040(8) C43 0.164(15) 0.160(15) 0.053(8) 0.031(8) 0.008(9) 0.036(12) C44 0.198(18) 0.157(15) 0.060(8) 0.036(9) 0.041(10) 0.074(14) C45 0.130(12) 0.120(11) 0.071(8) 0.014(8) 0.030(8) 0.038(9) C51 0.051(6) 0.063(7) 0.076(7) -0.007(5) 0.006(5) -0.002(5) C52 0.083(7) 0.055(7) 0.085(8) -0.005(6) 0.008(6) -0.019(6) C53 0.095(9) 0.081(9) 0.091(9) -0.008(7) 0.026(7) -0.021(7) C54 0.087(8) 0.057(7) 0.115(10) -0.024(7) -0.012(8) -0.005(6) C55 0.087(8) 0.081(9) 0.081(8) -0.017(6) 0.009(6) -0.013(7) C61 0.070(7) 0.060(6) 0.054(6) 0.004(5) 0.008(5) -0.009(5) C62 0.065(7) 0.089(8) 0.065(7) 0.002(6) 0.006(5) -0.003(6) C63 0.070(8) 0.130(11) 0.070(8) 0.007(8) -0.013(6) 0.009(7) C64 0.096(10) 0.152(13) 0.047(7) -0.020(8) -0.017(6) -0.002(9) C65 0.103(10) 0.118(10) 0.044(6) -0.004(6) -0.012(6) -0.001(8) C71 0.072(7) 0.057(6) 0.072(7) 0.000(5) 0.000(6) 0.000(5) C72 0.069(7) 0.110(10) 0.070(7) -0.009(7) -0.015(6) 0.006(7) C73 0.078(8) 0.138(12) 0.081(9) -0.001(8) -0.016(7) 0.012(8) C74 0.087(9) 0.131(12) 0.070(8) -0.010(8) -0.015(7) -0.015(8) C75 0.091(9) 0.108(10) 0.065(7) -0.019(7) -0.015(7) 0.002(7) C81 0.041(6) 0.091(8) 0.075(7) 0.020(6) 0.006(5) -0.003(5) C82 0.058(7) 0.120(11) 0.102(10) 0.026(8) 0.001(7) -0.008(7) C83 0.077(10) 0.166(17) 0.104(12) 0.026(11) 0.023(9) 0.006(10) C84 0.070(9) 0.175(17) 0.100(11) 0.047(11) 0.047(8) 0.031(10) C85 0.084(9) 0.111(10) 0.073(8) 0.002(7) 0.018(7) 0.035(7) C91 0.049(6) 0.076(7) 0.077(8) 0.012(6) 0.002(5) 0.003(5) C92 0.079(8) 0.063(7) 0.110(10) 0.020(7) 0.003(7) -0.007(6) C93 0.104(11) 0.104(11) 0.131(13) 0.060(11) -0.020(10) -0.031(8) C94 0.111(12) 0.193(19) 0.112(13) 0.077(13) -0.030(10) -0.071(12) C95 0.113(11) 0.171(16) 0.066(8) 0.024(9) -0.012(8) -0.017(11) C101 0.080(7) 0.060(7) 0.058(6) 0.001(5) 0.010(5) -0.001(5) C102 0.101(9) 0.090(9) 0.062(7) 0.003(6) 0.019(6) -0.009(7) C103 0.115(10) 0.068(8) 0.099(10) 0.010(7) 0.028(8) 0.004(7) C104 0.30(2) 0.070(9) 0.080(10) -0.001(8) 0.082(12) -0.038(12) C105 0.221(18) 0.102(11) 0.048(7) -0.017(7) 0.033(9) -0.032(11) C111 0.069(7) 0.056(6) 0.086(8) 0.001(6) 0.008(6) 0.003(5) C112 0.072(8) 0.079(8) 0.116(11) 0.008(8) -0.019(7) 0.009(6) C113 0.098(9) 0.077(9) 0.103(10) -0.021(8) 0.007(8) 0.017(7) C114 0.112(11) 0.087(10) 0.119(12) -0.045(9) 0.035(9) 0.010(8) C115 0.099(9) 0.063(7) 0.082(8) -0.014(6) 0.001(7) 0.003(6) C121 0.077(7) 0.050(6) 0.057(6) 0.003(4) 0.007(5) 0.009(5) C122 0.049(6) 0.114(10) 0.087(8) -0.004(7) -0.003(6) -0.004(6) C123 0.070(9) 0.152(14) 0.095(10) -0.008(9) -0.008(8) 0.008(8) C124 0.074(9) 0.149(14) 0.122(13) -0.018(11) 0.024(9) 0.029(9) C125 0.096(10) 0.131(12) 0.073(8) -0.001(8) 0.027(8) -0.005(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.108(7) . ? Ag1 N9 2.126(7) . ? Ag1 Ag5 2.7548(11) . ? Ag1 Ag2 2.9079(10) . ? Ag2 N6 2.106(8) . ? Ag2 N12 2.123(8) . ? Ag2 Ag3 2.7664(11) . ? Ag3 N66 2.168(9) . ? Ag3 N126 2.189(9) . ? Ag4 N76 2.167(9) . ? Ag4 N116 2.217(8) . ? Ag4 O4 2.554(6) . ? Ag5 N96 2.175(10) . ? Ag5 N36 2.182(9) . ? Ag5 O11' 2.460(11) . ? Ag6 N106 2.157(9) . ? Ag6 N26 2.223(9) . ? Ag6 O1 2.548(6) . ? Ag7 N56 2.172(8) . ? Ag7 N86 2.172(9) . ? Ag7 O3 2.513(7) . ? Ag8 N16 2.174(9) . ? Ag8 N46 2.201(9) . ? Ag8 O2 2.584(7) . ? P1 O1 1.475(7) . ? P1 N3 1.610(8) . ? P1 N1 1.649(8) . ? P1 N2 1.672(8) . ? P2 O2 1.458(7) . ? P2 N6 1.617(8) . ? P2 N5 1.661(8) . ? P2 N4 1.691(8) . ? P3 O3 1.471(7) . ? P3 N9 1.604(8) . ? P3 N7 1.662(8) . ? P3 N8 1.683(8) . ? P4 O4 1.477(7) . ? P4 N12 1.604(8) . ? P4 N10 1.664(8) . ? P4 N11 1.668(8) . ? N1 C11 1.417(12) . ? N2 C21 1.392(13) . ? N3 C31 1.416(12) . ? N4 C41 1.386(12) . ? N5 C51 1.407(12) . ? N6 C61 1.388(12) . ? N7 C71 1.399(12) . ? N8 C81 1.374(13) . ? N9 C91 1.386(12) . ? N10 C101 1.386(12) . ? N11 C111 1.376(13) . ? N12 C121 1.417(12) . ? N16 C15 1.314(14) . ? N16 C11 1.331(12) . ? N26 C21 1.290(13) . ? N26 C25 1.368(15) . ? N36 C35 1.310(14) . ? N36 C31 1.345(12) . ? N46 C41 1.355(13) . ? N46 C45 1.371(14) . ? N56 C51 1.332(12) . ? N56 C55 1.358(14) . ? N66 C65 1.347(14) . ? N66 C61 1.367(12) . ? N76 C71 1.354(13) . ? N76 C75 1.364(13) . ? N86 C81 1.322(14) . ? N86 C85 1.360(13) . ? N96 C91 1.354(14) . ? N96 C95 1.365(16) . ? N106 C101 1.346(13) . ? N106 C105 1.347(15) . ? N116 C111 1.324(13) . ? N116 C115 1.408(13) . ? N126 C125 1.331(15) . ? N126 C121 1.343(12) . ? C11 C12 1.399(14) . ? C12 C13 1.381(15) . ? C13 C14 1.387(16) . ? C14 C15 1.377(17) . ? C21 C22 1.410(16) . ? C22 C23 1.405(19) . ? C23 C24 1.34(2) . ? C24 C25 1.382(18) . ? C31 C32 1.390(14) . ? C32 C33 1.388(17) . ? C33 C34 1.347(19) . ? C34 C35 1.362(19) . ? C41 C42 1.384(15) . ? C42 C43 1.404(18) . ? C43 C44 1.334(19) . ? C44 C45 1.323(18) . ? C51 C52 1.366(14) . ? C52 C53 1.349(15) . ? C53 C54 1.382(16) . ? C54 C55 1.347(16) . ? C61 C62 1.387(14) . ? C62 C63 1.371(15) . ? C63 C64 1.348(17) . ? C64 C65 1.358(17) . ? C71 C72 1.353(14) . ? C72 C73 1.345(15) . ? C73 C74 1.418(18) . ? C74 C75 1.340(17) . ? C81 C82 1.432(15) . ? C82 C83 1.378(19) . ? C83 C84 1.37(2) . ? C84 C85 1.341(18) . ? C91 C92 1.404(15) . ? C92 C93 1.347(18) . ? C93 C94 1.30(2) . ? C94 C95 1.38(2) . ? C101 C102 1.372(15) . ? C102 C103 1.404(16) . ? C103 C104 1.334(19) . ? C104 C105 1.41(2) . ? C111 C112 1.435(15) . ? C112 C113 1.316(17) . ? C113 C114 1.387(19) . ? C114 C115 1.361(17) . ? C121 C122 1.358(14) . ? C122 C123 1.341(17) . ? C123 C124 1.365(19) . ? C124 C125 1.322(19) . ? Cl1 O12 1.444(4) . ? Cl1 O13 1.444(4) . ? Cl1 O14 1.444(4) . ? Cl1 O11 1.444(4) . ? Cl1' O11' 1.444(4) . ? Cl1' O14' 1.444(4) . ? Cl1' O13' 1.444(4) . ? Cl1' O12' 1.444(4) . ? O12' O43' 1.464(16) . ? Cl1" O12" 1.444(4) . ? Cl1" O14" 1.444(4) . ? Cl1" O11" 1.444(4) . ? Cl1" O13" 1.444(4) . ? Cl2 O21 1.444(4) . ? Cl2 O23 1.444(4) . ? Cl2 O24 1.444(4) . ? Cl2 O22 1.444(4) . ? Cl3 O32 1.444(4) . ? Cl3 O33 1.444(4) . ? Cl3 O34 1.444(4) . ? Cl3 O31 1.444(4) . ? Cl4 O43 1.444(4) . ? Cl4 O44 1.444(4) . ? Cl4 O42 1.444(4) . ? Cl4 O41 1.444(4) . ? Cl4' O42' 1.444(4) . ? Cl4' O41' 1.444(4) . ? Cl4' O44' 1.444(4) . ? Cl4' O43' 1.444(4) . ? Cl5 O53 1.444(4) . ? Cl5 O54 1.444(4) . ? Cl5 O52 1.444(4) . ? Cl5 O51 1.444(4) . ? O1S O3S 1.21(5) . ? O2S O3S 0.84(5) . ? O4S O5S 0.78(2) . ? O10S O11S 1.14(3) . ? O12S O12S 1.06(5) 2_554 ? 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 N9 164.0(3) . . ? N3 Ag1 Ag5 84.4(2) . . ? N9 Ag1 Ag5 80.1(2) . . ? N3 Ag1 Ag2 94.8(2) . . ? N9 Ag1 Ag2 100.1(2) . . ? Ag5 Ag1 Ag2 172.35(4) . . ? N6 Ag2 N12 163.3(3) . . ? N6 Ag2 Ag3 81.9(2) . . ? N12 Ag2 Ag3 81.4(2) . . ? N6 Ag2 Ag1 101.2(2) . . ? N12 Ag2 Ag1 95.3(2) . . ? Ag3 Ag2 Ag1 166.27(4) . . ? N66 Ag3 N126 162.5(3) . . ? N66 Ag3 Ag2 80.7(2) . . ? N126 Ag3 Ag2 81.9(2) . . ? N76 Ag4 N116 169.0(3) . . ? N76 Ag4 O4 100.0(3) . . ? N116 Ag4 O4 89.0(3) . . ? N96 Ag5 N36 161.5(3) . . ? N96 Ag5 O11' 94.9(5) . . ? N36 Ag5 O11' 98.5(5) . . ? N96 Ag5 Ag1 83.1(3) . . ? N36 Ag5 Ag1 79.0(2) . . ? O11' Ag5 Ag1 122.2(4) . . ? N106 Ag6 N26 168.6(4) . . ? N106 Ag6 O1 99.4(3) . . ? N26 Ag6 O1 88.0(3) . . ? N56 Ag7 N86 159.4(3) . . ? N56 Ag7 O3 102.5(3) . . ? N86 Ag7 O3 91.7(3) . . ? N16 Ag8 N46 162.9(3) . . ? N16 Ag8 O2 100.9(3) . . ? N46 Ag8 O2 88.0(3) . . ? O1 P1 N3 112.9(4) . . ? O1 P1 N1 110.6(4) . . ? N3 P1 N1 108.4(4) . . ? O1 P1 N2 111.3(4) . . ? N3 P1 N2 109.6(4) . . ? N1 P1 N2 103.6(4) . . ? O2 P2 N6 112.6(4) . . ? O2 P2 N5 112.2(4) . . ? N6 P2 N5 106.5(4) . . ? O2 P2 N4 113.0(4) . . ? N6 P2 N4 109.3(4) . . ? N5 P2 N4 102.7(4) . . ? O3 P3 N9 113.7(4) . . ? O3 P3 N7 111.3(4) . . ? N9 P3 N7 106.8(4) . . ? O3 P3 N8 111.2(4) . . ? N9 P3 N8 109.5(4) . . ? N7 P3 N8 103.6(4) . . ? O4 P4 N12 115.2(4) . . ? O4 P4 N10 109.4(4) . . ? N12 P4 N10 107.5(4) . . ? O4 P4 N11 110.6(4) . . ? N12 P4 N11 109.6(4) . . ? N10 P4 N11 103.9(4) . . ? P1 O1 Ag6 96.1(3) . . ? P2 O2 Ag8 93.8(3) . . ? P3 O3 Ag7 97.3(3) . . ? P4 O4 Ag4 98.1(3) . . ? C11 N1 P1 126.4(7) . . ? C21 N2 P1 129.1(7) . . ? C31 N3 P1 123.9(6) . . ? C31 N3 Ag1 115.1(6) . . ? P1 N3 Ag1 121.0(4) . . ? C41 N4 P2 126.9(7) . . ? C51 N5 P2 128.6(7) . . ? C61 N6 P2 121.7(7) . . ? C61 N6 Ag2 118.6(6) . . ? P2 N6 Ag2 119.2(4) . . ? C71 N7 P3 127.0(7) . . ? C81 N8 P3 126.6(7) . . ? C91 N9 P3 122.4(7) . . ? C91 N9 Ag1 119.9(6) . . ? P3 N9 Ag1 117.6(4) . . ? C101 N10 P4 125.8(7) . . ? C111 N11 P4 128.0(7) . . ? C121 N12 P4 123.6(6) . . ? C121 N12 Ag2 116.3(6) . . ? P4 N12 Ag2 119.5(4) . . ? C15 N16 C11 117.2(9) . . ? C15 N16 Ag8 117.0(8) . . ? C11 N16 Ag8 125.8(7) . . ? C21 N26 C25 116.8(10) . . ? C21 N26 Ag6 130.1(8) . . ? C25 N26 Ag6 112.9(8) . . ? C35 N36 C31 117.3(10) . . ? C35 N36 Ag5 116.3(8) . . ? C31 N36 Ag5 126.2(7) . . ? C41 N46 C45 113.3(9) . . ? C41 N46 Ag8 131.1(7) . . ? C45 N46 Ag8 115.5(8) . . ? C51 N56 C55 117.3(9) . . ? C51 N56 Ag7 124.8(7) . . ? C55 N56 Ag7 117.6(7) . . ? C65 N66 C61 119.0(10) . . ? C65 N66 Ag3 117.7(8) . . ? C61 N66 Ag3 123.3(7) . . ? C71 N76 C75 117.1(10) . . ? C71 N76 Ag4 126.1(7) . . ? C75 N76 Ag4 116.5(8) . . ? C81 N86 C85 117.2(10) . . ? C81 N86 Ag7 127.5(7) . . ? C85 N86 Ag7 114.8(9) . . ? C91 N96 C95 115.4(11) . . ? C91 N96 Ag5 121.6(7) . . ? C95 N96 Ag5 123.0(10) . . ? C101 N106 C105 118.1(10) . . ? C101 N106 Ag6 127.9(7) . . ? C105 N106 Ag6 114.1(8) . . ? C111 N116 C115 117.9(9) . . ? C111 N116 Ag4 130.0(7) . . ? C115 N116 Ag4 111.4(7) . . ? C125 N126 C121 118.8(10) . . ? C125 N126 Ag3 119.3(8) . . ? C121 N126 Ag3 121.7(7) . . ? N16 C11 C12 124.0(9) . . ? N16 C11 N1 116.5(9) . . ? C12 C11 N1 119.5(9) . . ? C13 C12 C11 115.9(11) . . ? C12 C13 C14 121.6(11) . . ? C15 C14 C13 116.0(11) . . ? N16 C15 C14 125.2(11) . . ? N26 C21 N2 120.0(9) . . ? N26 C21 C22 122.5(11) . . ? N2 C21 C22 117.5(11) . . ? C23 C22 C21 117.7(13) . . ? C24 C23 C22 121.5(14) . . ? C23 C24 C25 115.3(14) . . ? N26 C25 C24 126.0(13) . . ? N36 C31 C32 122.3(10) . . ? N36 C31 N3 116.3(8) . . ? C32 C31 N3 121.3(9) . . ? C33 C32 C31 117.5(12) . . ? C34 C33 C32 119.6(13) . . ? C33 C34 C35 118.8(12) . . ? N36 C35 C34 124.3(13) . . ? N46 C41 C42 123.9(10) . . ? N46 C41 N4 119.2(9) . . ? C42 C41 N4 116.8(10) . . ? C41 C42 C43 115.8(12) . . ? C44 C43 C42 123.1(13) . . ? C45 C44 C43 115.6(13) . . ? C44 C45 N46 128.4(13) . . ? N56 C51 C52 121.9(10) . . ? N56 C51 N5 114.9(9) . . ? C52 C51 N5 123.2(10) . . ? C53 C52 C51 119.5(11) . . ? C52 C53 C54 120.1(11) . . ? C55 C54 C53 117.3(11) . . ? C54 C55 N56 123.6(11) . . ? N66 C61 C62 118.1(10) . . ? N66 C61 N6 116.7(9) . . ? C62 C61 N6 125.1(10) . . ? C63 C62 C61 120.7(11) . . ? C64 C63 C62 120.3(12) . . ? C63 C64 C65 117.8(11) . . ? N66 C65 C64 123.7(12) . . ? C72 C71 N76 122.0(10) . . ? C72 C71 N7 123.6(10) . . ? N76 C71 N7 114.3(9) . . ? C73 C72 C71 121.4(12) . . ? C72 C73 C74 117.4(12) . . ? C75 C74 C73 119.3(12) . . ? C74 C75 N76 122.6(12) . . ? N86 C81 N8 122.0(9) . . ? N86 C81 C82 121.9(11) . . ? N8 C81 C82 115.9(12) . . ? C83 C82 C81 118.3(15) . . ? C84 C83 C82 118.4(15) . . ? C85 C84 C83 119.9(15) . . ? C84 C85 N86 123.9(15) . . ? N96 C91 N9 116.5(9) . . ? N96 C91 C92 121.1(11) . . ? N9 C91 C92 122.4(11) . . ? C93 C92 C91 120.0(14) . . ? C94 C93 C92 119.0(15) . . ? C93 C94 C95 121.6(15) . . ? N96 C95 C94 122.3(15) . . ? N106 C101 C102 122.1(10) . . ? N106 C101 N10 115.4(9) . . ? C102 C101 N10 122.5(10) . . ? C101 C102 C103 119.6(12) . . ? C104 C103 C102 118.4(13) . . ? C103 C104 C105 120.2(12) . . ? N106 C105 C104 121.5(12) . . ? N116 C111 N11 119.3(9) . . ? N116 C111 C112 119.6(11) . . ? N11 C111 C112 121.1(11) . . ? C113 C112 C111 122.8(13) . . ? C112 C113 C114 117.4(12) . . ? C115 C114 C113 120.7(12) . . ? C114 C115 N116 121.2(12) . . ? N126 C121 C122 119.8(10) . . ? N126 C121 N12 118.0(9) . . ? C122 C121 N12 122.2(10) . . ? C123 C122 C121 120.6(12) . . ? C122 C123 C124 118.5(13) . . ? C125 C124 C123 119.7(13) . . ? C124 C125 N126 122.3(13) . . ? O12 Cl1 O13 109.7(2) . . ? O12 Cl1 O14 109.0(4) . . ? O13 Cl1 O14 109.7(2) . . ? O12 Cl1 O11 109.7(2) . . ? O13 Cl1 O11 109.0(4) . . ? O14 Cl1 O11 109.7(2) . . ? O11' Cl1' O14' 109.8(2) . . ? O11' Cl1' O13' 109.0(4) . . ? O14' Cl1' O13' 109.7(2) . . ? O11' Cl1' O12' 109.7(2) . . ? O14' Cl1' O12' 108.9(4) . . ? O13' Cl1' O12' 109.7(2) . . ? Cl1' O11' Ag5 164.2(12) . . ? Cl1' O12' O43' 170.7(16) . . ? O12" Cl1" O14" 109.0(4) . . ? O12" Cl1" O11" 109.7(2) . . ? O14" Cl1" O11" 109.7(2) . . ? O12" Cl1" O13" 109.7(2) . . ? O14" Cl1" O13" 109.7(2) . . ? O11" Cl1" O13" 109.0(4) . . ? O21 Cl2 O23 109.0(4) . . ? O21 Cl2 O24 109.7(2) . . ? O23 Cl2 O24 109.7(2) . . ? O21 Cl2 O22 109.7(2) . . ? O23 Cl2 O22 109.7(2) . . ? O24 Cl2 O22 109.0(4) . . ? O32 Cl3 O33 109.7(2) . . ? O32 Cl3 O34 109.0(4) . . ? O33 Cl3 O34 109.7(2) . . ? O32 Cl3 O31 109.7(2) . . ? O33 Cl3 O31 109.0(4) . . ? O34 Cl3 O31 109.7(2) . . ? O43 Cl4 O44 109.7(2) . . ? O43 Cl4 O42 109.7(2) . . ? O44 Cl4 O42 109.0(4) . . ? O43 Cl4 O41 109.0(4) . . ? O44 Cl4 O41 109.7(2) . . ? O42 Cl4 O41 109.7(2) . . ? O42' Cl4' O41' 109.7(2) . . ? O42' Cl4' O44' 109.0(4) . . ? O41' Cl4' O44' 109.7(2) . . ? O42' Cl4' O43' 109.7(2) . . ? O41' Cl4' O43' 109.0(4) . . ? O44' Cl4' O43' 109.7(2) . . ? Cl4' O43' O12' 168.1(17) . . ? O53 Cl5 O54 109.7(2) . . ? O53 Cl5 O52 109.7(2) . . ? O54 Cl5 O52 109.0(4) . . ? O53 Cl5 O51 109.0(4) . . ? O54 Cl5 O51 109.7(2) . . ? O52 Cl5 O51 109.7(2) . . ? O2S O3S O1S 138(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.019 _refine_diff_density_min -1.295 _refine_diff_density_rms 0.131 # Attachment '- Compound4_new.cif' data_ag271054_0m _database_code_depnum_ccdc_archive 'CCDC 865265' #TrackingRef '- Compound4_new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H39 Ag7 N18 O3 P3 1+, B F4 1-, H2 O' _chemical_formula_sum 'C45 H41 Ag7 B F4 N18 O4 P3' _chemical_formula_weight 1832.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 14.1261(3) _cell_length_b 14.1261(3) _cell_length_c 24.5724(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4246.4(3) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 116 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 28.37 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2652 _exptl_absorpt_coefficient_mu 2.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Apex II' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_number 18418 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.47 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4402 _reflns_number_gt 3351 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. One pyridyl group is disordered. It was split over two positions and refined isotropically with occupancy factors and similar-distance and similar U restraints. Both the BF4 anion and the lattice water molecule are disordered over the 3-fold axis. The BF4 anion was refined isotropically with similar-distance and similar U-restraints. H-atoms of disordered water molecules were not added to the model. ; _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^)+(0.0560P)^2^+45.6120P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(7) _refine_ls_number_reflns 4402 _refine_ls_number_parameters 254 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.030 _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 0.85370(6) -0.03767(6) 0.60571(3) 0.04564(19) Uani 1 1 d . . . Ag2 Ag 0.86871(5) -0.09938(5) 0.71864(3) 0.03921(16) Uani 1 1 d . . . Ag3 Ag 1.0000 0.0000 0.81492(5) 0.0512(3) Uani 1 3 d S . . N1 N 0.8915(6) 0.1164(6) 0.6402(3) 0.0365(15) Uani 1 1 d . . . N2 N 0.8400(6) 0.0429(6) 0.7371(3) 0.0400(17) Uani 1 1 d . . . O1 O 0.6962(5) 0.0712(6) 0.6798(3) 0.0527(17) Uani 1 1 d . . . P1 P 0.81299(19) 0.11064(19) 0.69126(10) 0.0388(5) Uani 1 1 d . . . C11 C 0.9270(7) 0.1996(7) 0.6026(3) 0.0361(17) Uani 1 1 d . . . N12 N 1.0172(7) 0.2178(7) 0.5746(3) 0.0457(18) Uani 1 1 d . . . C13 C 1.0568(10) 0.2948(11) 0.5362(5) 0.061(3) Uani 1 1 d . . . H13 H 1.1190 0.3071 0.5173 0.073 Uiso 1 1 calc R . . C14 C 1.0104(12) 0.3564(11) 0.5233(5) 0.068(3) Uani 1 1 d . . . H14 H 1.0410 0.4105 0.4968 0.081 Uiso 1 1 calc R . . C15 C 0.9178(11) 0.3365(10) 0.5502(5) 0.065(3) Uani 1 1 d . . . H15 H 0.8842 0.3769 0.5420 0.077 Uiso 1 1 calc R . . C16 C 0.8750(9) 0.2582(8) 0.5889(5) 0.051(2) Uani 1 1 d . . . H16 H 0.8106 0.2433 0.6064 0.062 Uiso 1 1 calc R . . C21 C 0.7936(8) 0.0235(7) 0.7886(4) 0.043(2) Uani 1 1 d . . . N22 N 0.8413(8) -0.0041(8) 0.8283(4) 0.054(2) Uani 1 1 d . . . C23 C 0.7968(11) -0.0251(9) 0.8796(5) 0.065(3) Uani 1 1 d . . . H23 H 0.8302 -0.0443 0.9066 0.078 Uiso 1 1 calc R . . C24 C 0.7052(12) -0.0192(12) 0.8933(5) 0.081(4) Uani 1 1 d . . . H24 H 0.6773 -0.0330 0.9285 0.098 Uiso 1 1 calc R . . C25 C 0.6567(10) 0.0086(10) 0.8516(6) 0.069(4) Uani 1 1 d . . . H25 H 0.5942 0.0126 0.8589 0.083 Uiso 1 1 calc R . . C26 C 0.6991(9) 0.0297(9) 0.8009(5) 0.058(3) Uani 1 1 d . . . H26 H 0.6657 0.0485 0.7737 0.069 Uiso 1 1 calc R . . N3 N 0.8631(6) 0.2377(7) 0.7146(3) 0.048(2) Uani 1 1 d DU . . H3 H 0.8131 0.2520 0.7244 0.058 Uiso 1 1 calc R A 1 C31 C 0.9684(12) 0.3257(13) 0.7217(13) 0.047(8) Uiso 0.46(3) 1 d PDU B 1 N32 N 1.0516(11) 0.3052(12) 0.7211(10) 0.037(5) Uiso 0.46(3) 1 d PDU . 1 C33 C 1.1530(14) 0.3920(14) 0.7234(11) 0.044(5) Uiso 0.46(3) 1 d PDU B 1 H33 H 1.2112 0.3791 0.7209 0.053 Uiso 0.46(3) 1 calc PR B 1 C34 C 1.1763(16) 0.4951(16) 0.7290(11) 0.050(6) Uiso 0.46(3) 1 d PDU B 1 H34 H 1.2482 0.5525 0.7283 0.060 Uiso 0.46(3) 1 calc PR B 1 C35 C 1.0900(17) 0.5142(18) 0.7360(13) 0.064(7) Uiso 0.46(3) 1 d PDU B 1 H35 H 1.1038 0.5844 0.7438 0.077 Uiso 0.46(3) 1 calc PR B 1 C36 C 0.9849(16) 0.4306(15) 0.7315(13) 0.052(6) Uiso 0.46(3) 1 d PDU B 1 H36 H 0.9263 0.4428 0.7348 0.062 Uiso 0.46(3) 1 calc PR B 1 C31' C 0.9695(10) 0.3274(11) 0.7102(11) 0.039(6) Uiso 0.54(3) 1 d PDU B 2 N32' N 1.0518(11) 0.3049(12) 0.7070(9) 0.040(5) Uiso 0.54(3) 1 d PDU . 2 C33' C 1.1523(15) 0.3915(15) 0.7022(12) 0.060(6) Uiso 0.54(3) 1 d PDU B 2 H33' H 1.2105 0.3783 0.7020 0.072 Uiso 0.54(3) 1 calc PR B 2 C34' C 1.1761(17) 0.4954(18) 0.6976(12) 0.069(6) Uiso 0.54(3) 1 d PDU B 2 H34' H 1.2463 0.5511 0.6892 0.083 Uiso 0.54(3) 1 calc PR B 2 C35' C 1.0911(15) 0.5166(15) 0.7059(11) 0.058(6) Uiso 0.54(3) 1 d PDU B 2 H35' H 1.1063 0.5882 0.7105 0.070 Uiso 0.54(3) 1 calc PR B 2 C36' C 0.9864(14) 0.4336(13) 0.7074(11) 0.050(5) Uiso 0.54(3) 1 d PDU B 2 H36' H 0.9281 0.4467 0.7066 0.060 Uiso 0.54(3) 1 calc PR B 2 B1 B 0.6641(19) 0.329(2) 0.7893(8) 0.055(5) Uiso 0.33 1 d PD C -1 F1 F 0.691(3) 0.253(3) 0.8008(16) 0.166(18) Uiso 0.33 1 d PD C -1 F2 F 0.754(2) 0.424(2) 0.7756(13) 0.107(10) Uiso 0.33 1 d PD C -1 F3 F 0.594(3) 0.296(4) 0.7471(12) 0.171(17) Uiso 0.33 1 d PD C -1 F4 F 0.616(3) 0.344(3) 0.8333(10) 0.134(12) Uiso 0.33 1 d PD C -1 O2 O 0.627(3) 0.233(3) 0.6484(19) 0.118(14) Uani 0.33 1 d P . . 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 0.0582(5) 0.0389(4) 0.0424(3) -0.0053(3) -0.0025(3) 0.0262(3) Ag2 0.0363(3) 0.0336(3) 0.0476(4) -0.0034(3) 0.0027(3) 0.0173(3) Ag3 0.0599(5) 0.0599(5) 0.0338(6) 0.000 0.000 0.0300(2) N1 0.034(4) 0.033(4) 0.047(4) -0.003(3) 0.002(3) 0.020(3) N2 0.033(4) 0.033(4) 0.046(4) -0.014(3) 0.004(3) 0.010(3) O1 0.040(4) 0.069(5) 0.053(4) -0.016(3) -0.012(3) 0.031(3) P1 0.0328(11) 0.0429(12) 0.0438(12) -0.0112(10) -0.0029(9) 0.0212(10) C11 0.042(5) 0.041(5) 0.028(4) -0.004(3) -0.001(3) 0.022(4) N12 0.050(5) 0.052(5) 0.038(4) 0.002(3) 0.000(3) 0.028(4) C13 0.056(6) 0.072(8) 0.052(6) 0.017(5) 0.004(5) 0.030(6) C14 0.084(9) 0.069(8) 0.056(6) 0.023(6) 0.004(6) 0.042(7) C15 0.099(9) 0.060(7) 0.056(6) -0.003(5) -0.011(6) 0.055(7) C16 0.053(6) 0.053(6) 0.062(6) 0.003(5) -0.007(5) 0.037(5) C21 0.043(5) 0.026(4) 0.049(5) -0.006(4) 0.013(4) 0.009(4) N22 0.065(6) 0.052(5) 0.055(5) 0.002(4) 0.012(4) 0.036(5) C23 0.088(9) 0.059(7) 0.046(6) 0.003(5) 0.021(6) 0.034(6) C24 0.082(9) 0.081(9) 0.063(8) 0.003(7) 0.041(7) 0.027(8) C25 0.051(6) 0.070(8) 0.078(8) -0.024(7) 0.018(6) 0.024(6) C26 0.044(6) 0.057(6) 0.066(7) -0.022(5) 0.001(5) 0.022(5) N3 0.039(4) 0.056(5) 0.058(5) -0.017(4) -0.003(4) 0.030(4) O2 0.08(2) 0.09(2) 0.17(4) 0.01(2) -0.06(2) 0.039(19) _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 N12 2.139(8) 2_645 ? Ag1 N1 2.140(7) . ? Ag1 Ag2 2.9477(10) . ? Ag1 Ag1 3.2192(13) 2_645 ? Ag1 Ag1 3.2192(14) 3_765 ? Ag2 N2 2.286(7) . ? Ag2 N32 2.331(16) 2_645 ? Ag2 N32' 2.343(15) 2_645 ? Ag2 N2 2.393(7) 2_645 ? Ag2 Ag3 2.8990(12) . ? Ag2 Ag2 2.9018(11) 3_765 ? Ag2 Ag2 2.9019(11) 2_645 ? Ag2 P1 3.033(2) 2_645 ? Ag3 N22 2.238(9) . ? Ag3 N22 2.238(9) 3_765 ? Ag3 N22 2.238(9) 2_645 ? Ag3 Ag2 2.8990(12) 2_645 ? Ag3 Ag2 2.8990(12) 3_765 ? N1 C11 1.379(12) . ? N1 P1 1.649(7) . ? N2 C21 1.389(12) . ? N2 P1 1.641(9) . ? N2 Ag2 2.393(7) 3_765 ? O1 P1 1.480(7) . ? P1 N3 1.668(8) . ? P1 Ag2 3.033(2) 3_765 ? C11 N12 1.354(12) . ? C11 C16 1.396(12) . ? N12 C13 1.334(14) . ? N12 Ag1 2.139(8) 3_765 ? C13 C14 1.362(17) . ? C13 H13 0.9300 . ? C14 C15 1.364(18) . ? C14 H14 0.9300 . ? C15 C16 1.349(16) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 N22 1.348(14) . ? C21 C26 1.412(15) . ? N22 C23 1.375(13) . ? C23 C24 1.379(19) . ? C23 H23 0.9300 . ? C24 C25 1.39(2) . ? C24 H24 0.9300 . ? C25 C26 1.350(17) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? N3 C31 1.393(16) . ? N3 C31' 1.404(15) . ? N3 H3 0.8600 . ? C31 N32 1.344(16) . ? C31 C36 1.40(2) . ? N32 C33 1.342(18) . ? N32 Ag2 2.331(16) 3_765 ? C33 C34 1.33(2) . ? C33 H33 0.9300 . ? C34 C35 1.38(2) . ? C34 H34 0.9300 . ? C35 C36 1.36(2) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C31' N32' 1.352(15) . ? C31' C36' 1.398(19) . ? N32' C33' 1.337(18) . ? N32' Ag2 2.343(14) 3_765 ? C33' C34' 1.34(2) . ? C33' H33' 0.9300 . ? C34' C35' 1.39(2) . ? C34' H34' 0.9300 . ? C35' C36' 1.35(2) . ? C35' H35' 0.9300 . ? C36' H36' 0.9300 . ? B1 F4 1.345(17) . ? B1 F1 1.346(17) . ? B1 F2 1.347(17) . ? B1 F3 1.348(17) . ? 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 N12 Ag1 N1 168.3(3) 2_645 . ? N12 Ag1 Ag2 94.8(2) 2_645 . ? N1 Ag1 Ag2 84.8(2) . . ? N12 Ag1 Ag1 71.7(2) 2_645 2_645 ? N1 Ag1 Ag1 119.13(19) . 2_645 ? Ag2 Ag1 Ag1 73.70(2) . 2_645 ? N12 Ag1 Ag1 127.2(2) 2_645 3_765 ? N1 Ag1 Ag1 64.48(19) . 3_765 ? Ag2 Ag1 Ag1 91.256(18) . 3_765 ? Ag1 Ag1 Ag1 60.0 2_645 3_765 ? N2 Ag2 N32 104.4(4) . 2_645 ? N2 Ag2 N32' 106.0(4) . 2_645 ? N32 Ag2 N32' 8.5(7) 2_645 2_645 ? N2 Ag2 N2 151.1(4) . 2_645 ? N32 Ag2 N2 93.0(4) 2_645 2_645 ? N32' Ag2 N2 94.6(4) 2_645 2_645 ? N2 Ag2 Ag3 76.35(19) . . ? N32 Ag2 Ag3 123.5(6) 2_645 . ? N32' Ag2 Ag3 132.0(5) 2_645 . ? N2 Ag2 Ag3 74.8(2) 2_645 . ? N2 Ag2 Ag2 53.35(18) . 3_765 ? N32 Ag2 Ag2 157.5(3) 2_645 3_765 ? N32' Ag2 Ag2 156.4(3) 2_645 3_765 ? N2 Ag2 Ag2 108.77(19) 2_645 3_765 ? Ag3 Ag2 Ag2 59.967(15) . 3_765 ? N2 Ag2 Ag2 112.01(18) . 2_645 ? N32 Ag2 Ag2 142.4(3) 2_645 2_645 ? N32' Ag2 Ag2 142.0(3) 2_645 2_645 ? N2 Ag2 Ag2 50.02(18) 2_645 2_645 ? Ag3 Ag2 Ag2 59.967(15) . 2_645 ? Ag2 Ag2 Ag2 60.0 3_765 2_645 ? N2 Ag2 Ag1 81.7(2) . . ? N32 Ag2 Ag1 95.9(6) 2_645 . ? N32' Ag2 Ag1 87.8(5) 2_645 . ? N2 Ag2 Ag1 119.71(18) 2_645 . ? Ag3 Ag2 Ag1 138.44(3) . . ? Ag2 Ag2 Ag1 78.59(2) 3_765 . ? Ag2 Ag2 Ag1 97.925(19) 2_645 . ? N2 Ag2 P1 175.76(19) . 2_645 ? N32 Ag2 P1 71.7(4) 2_645 2_645 ? N32' Ag2 P1 69.9(3) 2_645 2_645 ? N2 Ag2 P1 32.6(2) 2_645 2_645 ? Ag3 Ag2 P1 107.13(5) . 2_645 ? Ag2 Ag2 P1 130.37(5) 3_765 2_645 ? Ag2 Ag2 P1 72.09(5) 2_645 2_645 ? Ag1 Ag2 P1 96.81(5) . 2_645 ? N22 Ag3 N22 117.89(12) . 3_765 ? N22 Ag3 N22 117.89(12) . 2_645 ? N22 Ag3 N22 117.89(12) 3_765 2_645 ? N22 Ag3 Ag2 132.3(2) . 2_645 ? N22 Ag3 Ag2 88.2(2) 3_765 2_645 ? N22 Ag3 Ag2 73.6(2) 2_645 2_645 ? N22 Ag3 Ag2 88.2(2) . 3_765 ? N22 Ag3 Ag2 73.6(2) 3_765 3_765 ? N22 Ag3 Ag2 132.3(2) 2_645 3_765 ? Ag2 Ag3 Ag2 60.07(3) 2_645 3_765 ? N22 Ag3 Ag2 73.6(2) . . ? N22 Ag3 Ag2 132.3(2) 3_765 . ? N22 Ag3 Ag2 88.2(2) 2_645 . ? Ag2 Ag3 Ag2 60.06(3) 2_645 . ? Ag2 Ag3 Ag2 60.06(3) 3_765 . ? C11 N1 P1 120.1(6) . . ? C11 N1 Ag1 113.6(5) . . ? P1 N1 Ag1 115.6(4) . . ? C21 N2 P1 121.0(7) . . ? C21 N2 Ag2 106.3(6) . . ? P1 N2 Ag2 124.9(4) . . ? C21 N2 Ag2 125.1(6) . 3_765 ? P1 N2 Ag2 95.7(3) . 3_765 ? Ag2 N2 Ag2 76.6(2) . 3_765 ? O1 P1 N2 116.8(4) . . ? O1 P1 N1 118.0(4) . . ? N2 P1 N1 101.7(4) . . ? O1 P1 N3 105.3(4) . . ? N2 P1 N3 107.1(4) . . ? N1 P1 N3 107.2(4) . . ? O1 P1 Ag2 165.7(3) . 3_765 ? N2 P1 Ag2 51.7(3) . 3_765 ? N1 P1 Ag2 62.3(3) . 3_765 ? N3 P1 Ag2 87.5(3) . 3_765 ? N12 C11 N1 114.2(7) . . ? N12 C11 C16 119.3(9) . . ? N1 C11 C16 126.3(9) . . ? C13 N12 C11 119.0(9) . . ? C13 N12 Ag1 122.2(7) . 3_765 ? C11 N12 Ag1 117.5(6) . 3_765 ? N12 C13 C14 123.1(11) . . ? N12 C13 H13 118.4 . . ? C14 C13 H13 118.4 . . ? C13 C14 C15 118.3(11) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C16 C15 C14 120.1(11) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 120.1(11) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? N22 C21 N2 117.4(9) . . ? N22 C21 C26 119.2(9) . . ? N2 C21 C26 123.4(10) . . ? C21 N22 C23 119.0(10) . . ? C21 N22 Ag3 121.7(6) . . ? C23 N22 Ag3 119.0(8) . . ? N22 C23 C24 123.5(13) . . ? N22 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C25 116.5(11) . . ? C23 C24 H24 121.7 . . ? C25 C24 H24 121.7 . . ? C26 C25 C24 121.0(12) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C21 120.8(12) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C31 N3 C31' 11.7(19) . . ? C31 N3 P1 133.9(10) . . ? C31' N3 P1 129.1(9) . . ? C31 N3 H3 113.1 . . ? C31' N3 H3 116.4 . . ? P1 N3 H3 113.1 . . ? N32 C31 N3 117.7(14) . . ? N32 C31 C36 121.9(14) . . ? N3 C31 C36 120.3(14) . . ? C33 N32 C31 116.8(14) . . ? C33 N32 Ag2 118.4(11) . 3_765 ? C31 N32 Ag2 124.8(11) . 3_765 ? C34 C33 N32 124.9(17) . . ? C34 C33 H33 117.5 . . ? N32 C33 H33 117.5 . . ? C33 C34 C35 117.7(17) . . ? C33 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? C36 C35 C34 120.4(19) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C31 117.6(17) . . ? C35 C36 H36 121.2 . . ? C31 C36 H36 121.2 . . ? N32' C31' C36' 122.9(13) . . ? N32' C31' N3 116.8(12) . . ? C36' C31' N3 120.3(12) . . ? C33' N32' C31' 115.8(13) . . ? C33' N32' Ag2 119.0(11) . 3_765 ? C31' N32' Ag2 124.9(10) . 3_765 ? N32' C33' C34' 125.5(17) . . ? N32' C33' H33' 117.3 . . ? C34' C33' H33' 117.3 . . ? C33' C34' C35' 117.0(18) . . ? C33' C34' H34' 121.5 . . ? C35' C34' H34' 121.5 . . ? C36' C35' C34' 120.4(18) . . ? C36' C35' H35' 119.8 . . ? C34' C35' H35' 119.8 . . ? C35' C36' C31' 117.2(15) . . ? C35' C36' H36' 121.4 . . ? C31' C36' H36' 121.4 . . ? F4 B1 F1 108.7(10) . . ? F4 B1 F2 110.2(10) . . ? F1 B1 F2 110.3(11) . . ? F4 B1 F3 109.5(10) . . ? F1 B1 F3 109.5(11) . . ? F2 B1 F3 108.5(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.181 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.155 # Attachment '- compound3a_new_squeeze.cif' data_compound3a_new_squeeze _database_code_depnum_ccdc_archive 'CCDC 882870' #TrackingRef '- compound3a_new_squeeze.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H54 Ag8 N24 O4 P4 4+, (Cl O4 1-)4, (C H4 O)5, (H2 O)3' _chemical_formula_sum 'C65 H80 Ag8 Cl4 N24 O28 P4' _chemical_formula_weight 2774.17 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.075(3) _cell_length_b 13.2864(7) _cell_length_c 27.6363(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.737(2) _cell_angle_gamma 90.00 _cell_volume 18018.2(17) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 147 _cell_measurement_theta_min 4.10 _cell_measurement_theta_max 25.03 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 2.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10928 _exptl_absorpt_coefficient_mu 1.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6356 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Apex II' _diffrn_measurement_method 'Omega and phi scans' _diffrn_reflns_number 104100 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 25.03 _reflns_number_total 15842 _reflns_number_gt 9115 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.005 1000 501 ' ' 2 0.250 0.777 -0.001 1795 949 ' ' 3 0.500 0.500 -0.006 999 500 ' ' 4 0.750 0.277 -0.001 1795 949 ' ' _platon_squeeze_details ; The unit cell contains 4 perchlorate ions, 5 methanol and three water molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _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^)+(0.0500P)^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_number_reflns 15842 _refine_ls_number_parameters 903 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1121 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.127722(8) 0.36079(3) -0.018083(15) 0.06168(14) Uani 1 1 d . . . Ag2 Ag 0.110066(9) 0.40468(3) 0.079731(15) 0.06469(14) Uani 1 1 d . . . Ag3 Ag 0.103429(10) 0.47898(4) 0.172254(16) 0.08027(16) Uani 1 1 d . . . Ag4 Ag 0.136996(10) 0.67285(4) 0.119022(17) 0.07906(16) Uani 1 1 d . . . Ag5 Ag 0.147191(11) 0.29581(4) -0.105654(18) 0.09008(18) Uani 1 1 d . . . Ag6 Ag 0.079451(12) 0.41987(4) -0.118123(18) 0.0968(2) Uani 1 1 d . . . Ag7 Ag 0.192385(12) 0.21000(4) -0.01767(2) 0.0963(2) Uani 1 1 d . . . Ag8 Ag 0.069636(11) 0.23757(5) 0.145137(18) 0.1012(2) Uani 1 1 d . . . P1 P 0.06317(3) 0.30869(12) -0.02529(5) 0.0557(4) Uani 1 1 d . . . P2 P 0.12234(3) 0.16955(11) 0.09779(5) 0.0576(4) Uani 1 1 d . . . P3 P 0.18511(3) 0.41497(11) 0.03178(5) 0.0558(4) Uani 1 1 d . . . P4 P 0.10486(3) 0.61775(11) 0.02425(5) 0.0565(4) Uani 1 1 d . . . O1 O 0.05968(7) 0.4174(3) -0.03328(12) 0.0620(10) Uani 1 1 d . . . O2 O 0.09552(7) 0.1564(3) 0.07440(13) 0.0660(10) Uani 1 1 d . . . O3 O 0.18188(6) 0.3157(2) 0.05531(12) 0.0592(9) Uani 1 1 d . . . O4 O 0.13510(7) 0.6265(3) 0.02955(12) 0.0610(9) Uani 1 1 d . . . N1 N 0.05518(9) 0.2786(3) 0.03065(15) 0.0631(12) Uani 1 1 d . . . H1A H 0.0650 0.2328 0.0444 0.076 Uiso 1 1 calc R . . N2 N 0.04078(8) 0.2404(3) -0.05835(16) 0.0627(12) Uani 1 1 d . . . H2 H 0.0285 0.2094 -0.0421 0.075 Uiso 1 1 calc R . . N3 N 0.09345(8) 0.2698(3) -0.03592(15) 0.0557(11) Uani 1 1 d . . . N4 N 0.12783(8) 0.0857(3) 0.14248(15) 0.0613(12) Uani 1 1 d . . . H4A H 0.1396 0.0394 0.1369 0.074 Uiso 1 1 calc R . . N5 N 0.14752(8) 0.1475(3) 0.06032(15) 0.0574(11) Uani 1 1 d . . . H5 H 0.1591 0.1957 0.0570 0.069 Uiso 1 1 calc R . . N6 N 0.12679(8) 0.2817(3) 0.11794(15) 0.0532(11) Uani 1 1 d . . . N7 N 0.17709(8) 0.5074(3) 0.06937(15) 0.0609(12) Uani 1 1 d . . . H7 H 0.1650 0.5492 0.0589 0.073 Uiso 1 1 calc R . . N8 N 0.21801(8) 0.4385(3) 0.01885(16) 0.0636(12) Uani 1 1 d . . . H8A H 0.2262 0.4817 0.0371 0.076 Uiso 1 1 calc R . . N9 N 0.16655(8) 0.4278(3) -0.01614(15) 0.0564(11) Uani 1 1 d . . . N10 N 0.09701(8) 0.5795(3) -0.03096(15) 0.0615(12) Uani 1 1 d . . . H10 H 0.0846 0.5341 -0.0333 0.074 Uiso 1 1 calc R . . N11 N 0.09007(9) 0.7310(3) 0.02748(16) 0.0625(12) Uani 1 1 d . . . H11 H 0.0841 0.7555 0.0006 0.075 Uiso 1 1 calc R . . N12 N 0.09066(9) 0.5428(3) 0.06172(15) 0.0575(11) Uani 1 1 d . . . N16 N 0.03634(9) 0.3109(4) 0.10633(18) 0.0739(14) Uani 1 1 d . . . N26 N 0.05258(10) 0.2910(4) -0.13705(19) 0.0783(14) Uani 1 1 d . . . N36 N 0.12030(9) 0.1714(4) -0.08646(16) 0.0665(13) Uani 1 1 d . . . N46 N 0.09312(11) 0.1384(4) 0.19508(17) 0.0759(14) Uani 1 1 d . . . N56 N 0.17073(9) 0.0710(3) -0.00203(17) 0.0643(12) Uani 1 1 d . . . N66 N 0.13815(10) 0.3834(4) 0.18532(17) 0.0696(13) Uani 1 1 d . . . N76 N 0.17523(9) 0.5999(4) 0.13978(17) 0.0709(13) Uani 1 1 d . . . N86 N 0.22514(10) 0.3089(4) -0.03849(18) 0.0744(14) Uani 1 1 d . . . N96 N 0.17212(10) 0.4323(4) -0.09989(19) 0.0786(15) Uani 1 1 d . . . N106 N 0.10314(12) 0.5584(4) -0.1130(2) 0.0924(17) Uani 1 1 d . . . N116 N 0.10062(10) 0.7696(3) 0.10879(18) 0.0678(13) Uani 1 1 d . . . N126 N 0.06950(10) 0.5555(4) 0.13719(17) 0.0728(14) Uani 1 1 d . . . C11 C 0.03408(11) 0.3199(4) 0.0583(2) 0.0620(15) Uani 1 1 d . . . C12 C 0.01213(12) 0.3679(5) 0.0356(2) 0.0748(17) Uani 1 1 d . . . H12 H 0.0111 0.3728 0.0020 0.090 Uiso 1 1 calc R . . C13 C -0.00782(12) 0.4077(5) 0.0641(3) 0.087(2) Uani 1 1 d . . . H13 H -0.0227 0.4405 0.0502 0.105 Uiso 1 1 calc R . . C14 C -0.00554(13) 0.3986(5) 0.1144(3) 0.090(2) Uani 1 1 d . . . H14 H -0.0186 0.4262 0.1345 0.108 Uiso 1 1 calc R . . C15 C 0.01586(15) 0.3492(6) 0.1326(2) 0.098(2) Uani 1 1 d . . . H15 H 0.0167 0.3405 0.1660 0.118 Uiso 1 1 calc R . . C21 C 0.03941(12) 0.2273(5) -0.1082(2) 0.0704(17) Uani 1 1 d . . . C22 C 0.02379(14) 0.1472(6) -0.1275(3) 0.102(2) Uani 1 1 d . . . H22 H 0.0144 0.1046 -0.1068 0.122 Uiso 1 1 calc R . . C23 C 0.02227(18) 0.1318(8) -0.1762(4) 0.137(3) Uani 1 1 d . . . H23 H 0.0130 0.0765 -0.1889 0.164 Uiso 1 1 calc R . . C24 C 0.03465(19) 0.1995(7) -0.2059(3) 0.118(3) Uani 1 1 d . . . H24 H 0.0327 0.1938 -0.2393 0.142 Uiso 1 1 calc R . . C25 C 0.04997(16) 0.2762(6) -0.1863(3) 0.107(2) Uani 1 1 d . . . H25 H 0.0589 0.3198 -0.2071 0.129 Uiso 1 1 calc R . . C31 C 0.09960(11) 0.1743(4) -0.05477(19) 0.0549(14) Uani 1 1 d . . . C32 C 0.08590(13) 0.0892(5) -0.0411(2) 0.0730(17) Uani 1 1 d . . . H32 H 0.0727 0.0924 -0.0172 0.088 Uiso 1 1 calc R . . C33 C 0.09183(17) -0.0009(6) -0.0629(3) 0.095(2) Uani 1 1 d . . . H33 H 0.0823 -0.0590 -0.0550 0.114 Uiso 1 1 calc R . . C34 C 0.11223(19) -0.0038(6) -0.0969(3) 0.102(2) Uani 1 1 d . . . H34 H 0.1163 -0.0633 -0.1129 0.122 Uiso 1 1 calc R . . C35 C 0.12624(15) 0.0823(6) -0.1063(2) 0.090(2) Uani 1 1 d . . . H35 H 0.1407 0.0791 -0.1277 0.108 Uiso 1 1 calc R . . C41 C 0.11546(13) 0.0830(4) 0.1872(2) 0.0643(15) Uani 1 1 d . . . C42 C 0.12610(15) 0.0183(5) 0.2217(2) 0.098(2) Uani 1 1 d . . . H42 H 0.1415 -0.0201 0.2153 0.118 Uiso 1 1 calc R . . C43 C 0.1134(2) 0.0120(7) 0.2656(3) 0.131(3) Uani 1 1 d . . . H43 H 0.1204 -0.0307 0.2894 0.157 Uiso 1 1 calc R . . C44 C 0.0909(2) 0.0672(7) 0.2747(3) 0.145(4) Uani 1 1 d . . . H44 H 0.0823 0.0640 0.3045 0.174 Uiso 1 1 calc R . . C45 C 0.08126(17) 0.1271(6) 0.2388(3) 0.110(3) Uani 1 1 d . . . H45 H 0.0654 0.1631 0.2445 0.132 Uiso 1 1 calc R . . C51 C 0.15258(11) 0.0607(5) 0.0333(2) 0.0615(15) Uani 1 1 d . . . C52 C 0.14067(13) -0.0314(5) 0.0418(2) 0.0760(17) Uani 1 1 d . . . H52 H 0.1272 -0.0373 0.0650 0.091 Uiso 1 1 calc R . . C53 C 0.14873(15) -0.1135(5) 0.0164(3) 0.087(2) Uani 1 1 d . . . H53 H 0.1410 -0.1760 0.0227 0.105 Uiso 1 1 calc R . . C54 C 0.16793(14) -0.1049(5) -0.0183(3) 0.0842(19) Uani 1 1 d . . . H54 H 0.1739 -0.1610 -0.0353 0.101 Uiso 1 1 calc R . . C55 C 0.17815(13) -0.0123(6) -0.0274(2) 0.0847(19) Uani 1 1 d . . . H55 H 0.1908 -0.0053 -0.0520 0.102 Uiso 1 1 calc R . . C61 C 0.14430(12) 0.3028(4) 0.1566(2) 0.0586(15) Uani 1 1 d . . . C62 C 0.16787(12) 0.2472(5) 0.1679(2) 0.0714(16) Uani 1 1 d . . . H62 H 0.1730 0.1954 0.1473 0.086 Uiso 1 1 calc R . . C63 C 0.18358(14) 0.2660(6) 0.2081(2) 0.092(2) Uani 1 1 d . . . H63 H 0.1985 0.2256 0.2156 0.111 Uiso 1 1 calc R . . C64 C 0.17693(16) 0.3448(7) 0.2369(2) 0.103(2) Uani 1 1 d . . . H64 H 0.1872 0.3597 0.2645 0.123 Uiso 1 1 calc R . . C65 C 0.15422(16) 0.4034(6) 0.2238(2) 0.091(2) Uani 1 1 d . . . H65 H 0.1501 0.4589 0.2429 0.109 Uiso 1 1 calc R . . C71 C 0.18732(12) 0.5258(4) 0.1151(2) 0.0622(15) Uani 1 1 d . . . C72 C 0.20902(13) 0.4748(5) 0.1339(2) 0.0828(19) Uani 1 1 d . . . H72 H 0.2167 0.4222 0.1166 0.099 Uiso 1 1 calc R . . C73 C 0.21959(14) 0.5002(6) 0.1779(3) 0.100(2) Uani 1 1 d . . . H73 H 0.2342 0.4645 0.1912 0.120 Uiso 1 1 calc R . . C74 C 0.20811(16) 0.5809(7) 0.2028(3) 0.105(2) Uani 1 1 d . . . H74 H 0.2154 0.6022 0.2323 0.126 Uiso 1 1 calc R . . C75 C 0.18582(14) 0.6282(5) 0.1829(2) 0.090(2) Uani 1 1 d . . . H75 H 0.1778 0.6810 0.1996 0.108 Uiso 1 1 calc R . . C81 C 0.23330(12) 0.3964(5) -0.0176(2) 0.0707(17) Uani 1 1 d . . . C82 C 0.25662(13) 0.4481(6) -0.0320(3) 0.099(2) Uani 1 1 d . . . H82 H 0.2620 0.5078 -0.0171 0.119 Uiso 1 1 calc R . . C83 C 0.27151(15) 0.4066(9) -0.0697(3) 0.113(3) Uani 1 1 d . . . H83 H 0.2870 0.4393 -0.0806 0.136 Uiso 1 1 calc R . . C84 C 0.26345(18) 0.3177(9) -0.0907(3) 0.117(3) Uani 1 1 d . . . H84 H 0.2735 0.2895 -0.1156 0.140 Uiso 1 1 calc R . . C85 C 0.24086(14) 0.2722(5) -0.0750(2) 0.088(2) Uani 1 1 d . . . H85 H 0.2356 0.2122 -0.0898 0.106 Uiso 1 1 calc R . . C91 C 0.17624(11) 0.4780(5) -0.0572(2) 0.0644(15) Uani 1 1 d . . . C92 C 0.18986(12) 0.5696(5) -0.0542(3) 0.085(2) Uani 1 1 d . . . H92 H 0.1907 0.6043 -0.0250 0.102 Uiso 1 1 calc R . . C93 C 0.20216(17) 0.6091(7) -0.0948(4) 0.123(3) Uani 1 1 d . . . H93 H 0.2121 0.6686 -0.0928 0.148 Uiso 1 1 calc R . . C94 C 0.19956(19) 0.5596(9) -0.1374(4) 0.146(4) Uani 1 1 d . . . H94 H 0.2081 0.5837 -0.1649 0.175 Uiso 1 1 calc R . . C95 C 0.18382(16) 0.4714(7) -0.1395(3) 0.117(3) Uani 1 1 d . . . H95 H 0.1814 0.4390 -0.1691 0.141 Uiso 1 1 calc R . . C101 C 0.10825(12) 0.6124(5) -0.0743(2) 0.0646(15) Uani 1 1 d . . . C102 C 0.12449(13) 0.6958(5) -0.0764(2) 0.0795(18) Uani 1 1 d . . . H102 H 0.1285 0.7318 -0.0483 0.095 Uiso 1 1 calc R . . C103 C 0.13501(14) 0.7268(5) -0.1199(3) 0.089(2) Uani 1 1 d . . . H103 H 0.1460 0.7837 -0.1217 0.107 Uiso 1 1 calc R . . C104 C 0.12904(19) 0.6739(6) -0.1590(3) 0.121(3) Uani 1 1 d . . . H104 H 0.1356 0.6939 -0.1889 0.145 Uiso 1 1 calc R . . C105 C 0.11370(19) 0.5923(6) -0.1559(3) 0.128(3) Uani 1 1 d . . . H105 H 0.1099 0.5562 -0.1840 0.154 Uiso 1 1 calc R . . C111 C 0.08628(12) 0.7900(4) 0.0679(2) 0.0691(16) Uani 1 1 d . . . C112 C 0.06682(13) 0.8681(5) 0.0663(3) 0.089(2) Uani 1 1 d . . . H112 H 0.0577 0.8829 0.0374 0.107 Uiso 1 1 calc R . . C113 C 0.06153(14) 0.9215(5) 0.1070(3) 0.094(2) Uani 1 1 d . . . H113 H 0.0489 0.9737 0.1062 0.113 Uiso 1 1 calc R . . C114 C 0.07507(15) 0.8974(5) 0.1496(3) 0.093(2) Uani 1 1 d . . . H114 H 0.0708 0.9303 0.1783 0.112 Uiso 1 1 calc R . . C115 C 0.09495(14) 0.8240(5) 0.1491(2) 0.0796(18) Uani 1 1 d . . . H115 H 0.1048 0.8112 0.1773 0.096 Uiso 1 1 calc R . . C121 C 0.06809(13) 0.5683(4) 0.0896(2) 0.0629(15) Uani 1 1 d . . . C122 C 0.04499(13) 0.6080(5) 0.0674(2) 0.0830(19) Uani 1 1 d . . . H122 H 0.0436 0.6134 0.0339 0.100 Uiso 1 1 calc R . . C123 C 0.02421(15) 0.6393(6) 0.0971(4) 0.112(3) Uani 1 1 d . . . H123 H 0.0085 0.6665 0.0832 0.134 Uiso 1 1 calc R . . C124 C 0.02619(16) 0.6313(6) 0.1459(3) 0.109(3) Uani 1 1 d . . . H124 H 0.0125 0.6553 0.1657 0.131 Uiso 1 1 calc R . . C125 C 0.04835(17) 0.5879(6) 0.1643(3) 0.098(2) Uani 1 1 d . . . H125 H 0.0495 0.5791 0.1976 0.117 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 0.0499(3) 0.0744(3) 0.0608(3) -0.0068(2) 0.0038(2) -0.0070(2) Ag2 0.0832(3) 0.0591(3) 0.0518(3) 0.0047(2) 0.0040(2) 0.0050(2) Ag3 0.1006(4) 0.0857(4) 0.0547(3) 0.0002(2) 0.0051(3) 0.0139(3) Ag4 0.0878(4) 0.0824(4) 0.0667(3) -0.0095(3) -0.0099(3) 0.0199(3) Ag5 0.0940(4) 0.1134(4) 0.0632(3) -0.0138(3) 0.0144(3) -0.0206(3) Ag6 0.1335(5) 0.0914(4) 0.0659(3) -0.0094(3) 0.0130(3) -0.0357(3) Ag7 0.1102(4) 0.0831(4) 0.0965(4) -0.0200(3) 0.0404(3) -0.0299(3) Ag8 0.0949(4) 0.1397(5) 0.0694(3) 0.0263(3) 0.0130(3) 0.0415(4) P1 0.0447(9) 0.0666(11) 0.0558(9) 0.0026(7) -0.0019(7) -0.0035(7) P2 0.0572(10) 0.0568(10) 0.0589(9) 0.0073(7) 0.0038(8) -0.0031(7) P3 0.0474(9) 0.0593(10) 0.0608(10) -0.0028(7) 0.0048(7) -0.0046(7) P4 0.0636(10) 0.0551(10) 0.0507(9) 0.0002(7) -0.0053(7) 0.0037(7) O1 0.059(2) 0.069(3) 0.057(2) 0.0060(18) -0.0004(18) -0.0015(19) O2 0.067(3) 0.064(3) 0.067(2) 0.0052(19) 0.002(2) -0.0071(19) O3 0.053(2) 0.051(2) 0.074(3) 0.0025(18) 0.0131(18) -0.0021(17) O4 0.066(3) 0.060(2) 0.057(2) -0.0037(18) -0.0066(18) 0.0008(18) N1 0.059(3) 0.073(3) 0.058(3) 0.007(2) 0.002(2) 0.008(2) N2 0.047(3) 0.087(3) 0.054(3) -0.005(2) -0.001(2) -0.013(2) N3 0.046(3) 0.060(3) 0.061(3) -0.001(2) 0.000(2) -0.005(2) N4 0.063(3) 0.063(3) 0.058(3) 0.008(2) 0.011(2) 0.010(2) N5 0.055(3) 0.048(3) 0.069(3) -0.005(2) 0.007(2) -0.005(2) N6 0.054(3) 0.054(3) 0.052(3) 0.006(2) -0.003(2) -0.003(2) N7 0.064(3) 0.064(3) 0.055(3) -0.009(2) -0.009(2) 0.011(2) N8 0.041(3) 0.079(3) 0.070(3) -0.005(3) -0.002(2) -0.015(2) N9 0.050(3) 0.061(3) 0.058(3) -0.003(2) 0.003(2) -0.007(2) N10 0.061(3) 0.070(3) 0.053(3) 0.007(2) -0.003(2) -0.023(2) N11 0.074(3) 0.060(3) 0.054(3) 0.005(2) -0.005(2) 0.010(2) N12 0.070(3) 0.052(3) 0.050(3) 0.002(2) 0.003(2) 0.007(2) N16 0.059(3) 0.110(4) 0.053(3) 0.013(3) 0.016(3) 0.008(3) N26 0.079(4) 0.088(4) 0.068(4) -0.005(3) 0.006(3) -0.010(3) N36 0.068(3) 0.080(4) 0.052(3) -0.011(3) 0.002(3) 0.007(3) N46 0.086(4) 0.086(4) 0.055(3) 0.010(3) 0.009(3) 0.012(3) N56 0.061(3) 0.060(3) 0.071(3) -0.011(3) -0.002(3) -0.007(2) N66 0.079(3) 0.076(4) 0.054(3) 0.003(3) 0.004(3) -0.004(3) N76 0.072(3) 0.089(4) 0.051(3) -0.004(3) -0.005(3) 0.002(3) N86 0.067(3) 0.085(4) 0.072(4) 0.013(3) 0.011(3) 0.005(3) N96 0.079(4) 0.101(4) 0.056(3) 0.021(3) 0.001(3) -0.010(3) N106 0.151(5) 0.067(4) 0.060(4) -0.005(3) 0.015(3) -0.020(3) N116 0.083(4) 0.062(3) 0.058(3) -0.005(3) -0.001(3) 0.007(3) N126 0.085(4) 0.086(4) 0.048(3) 0.003(3) 0.002(3) 0.007(3) C11 0.048(4) 0.074(4) 0.064(4) 0.006(3) 0.021(3) 0.003(3) C12 0.051(4) 0.097(5) 0.077(4) 0.011(4) 0.010(3) 0.012(3) C13 0.045(4) 0.127(6) 0.090(5) 0.000(4) 0.003(4) 0.010(4) C14 0.059(4) 0.126(6) 0.087(6) -0.008(4) 0.020(4) 0.014(4) C15 0.075(5) 0.154(7) 0.065(4) 0.011(4) 0.024(4) 0.028(5) C21 0.059(4) 0.073(5) 0.079(5) -0.005(4) -0.014(3) 0.001(3) C22 0.105(6) 0.109(6) 0.090(6) -0.001(5) -0.020(4) -0.034(5) C23 0.133(8) 0.164(9) 0.113(8) -0.028(7) -0.031(6) -0.049(7) C24 0.131(7) 0.131(8) 0.091(6) -0.053(6) -0.026(5) -0.006(6) C25 0.122(6) 0.141(7) 0.059(5) -0.017(5) 0.018(4) -0.019(5) C31 0.059(4) 0.057(4) 0.049(3) -0.004(3) -0.010(3) -0.005(3) C32 0.080(4) 0.063(5) 0.076(4) -0.002(4) -0.002(3) -0.007(4) C33 0.117(6) 0.071(6) 0.097(6) 0.007(4) -0.012(5) -0.012(4) C34 0.138(7) 0.075(6) 0.092(6) -0.027(4) -0.017(5) 0.019(5) C35 0.094(5) 0.092(6) 0.083(5) -0.030(4) -0.006(4) 0.015(5) C41 0.079(4) 0.063(4) 0.051(4) 0.004(3) -0.004(3) 0.006(3) C42 0.119(6) 0.114(6) 0.063(5) 0.017(4) -0.004(4) 0.032(5) C43 0.192(9) 0.137(7) 0.063(5) 0.030(5) 0.015(6) 0.064(7) C44 0.228(11) 0.147(8) 0.061(5) 0.029(5) 0.040(6) 0.076(8) C45 0.146(7) 0.118(6) 0.066(5) 0.018(5) 0.031(5) 0.042(5) C51 0.049(4) 0.075(5) 0.061(4) 0.001(3) 0.002(3) -0.012(3) C52 0.084(5) 0.056(4) 0.088(5) 0.007(4) 0.011(4) -0.016(4) C53 0.097(5) 0.067(5) 0.098(5) -0.011(4) 0.008(4) -0.017(4) C54 0.085(5) 0.060(5) 0.107(6) -0.024(4) 0.002(4) -0.012(4) C55 0.079(5) 0.085(5) 0.090(5) -0.023(4) 0.007(4) -0.011(4) C61 0.066(4) 0.051(4) 0.059(4) 0.013(3) 0.016(3) 0.000(3) C62 0.070(4) 0.083(5) 0.062(4) -0.002(3) 0.014(3) -0.005(4) C63 0.084(5) 0.130(6) 0.061(5) -0.008(4) -0.011(4) 0.013(4) C64 0.104(6) 0.155(8) 0.049(4) -0.011(5) -0.010(4) -0.007(6) C65 0.114(6) 0.114(6) 0.044(4) -0.016(4) -0.006(4) 0.000(5) C71 0.064(4) 0.059(4) 0.064(4) 0.000(3) 0.003(3) 0.006(3) C72 0.074(5) 0.101(5) 0.072(5) -0.010(4) -0.010(4) 0.011(4) C73 0.079(5) 0.136(7) 0.084(5) 0.010(5) -0.012(4) 0.023(5) C74 0.085(5) 0.163(8) 0.065(5) -0.020(5) -0.015(4) -0.001(5) C75 0.086(5) 0.116(6) 0.068(5) -0.014(4) -0.011(4) 0.007(4) C81 0.046(4) 0.090(5) 0.077(5) 0.025(4) 0.007(3) 0.004(4) C82 0.053(4) 0.140(7) 0.105(6) 0.025(5) 0.014(4) -0.008(4) C83 0.058(5) 0.176(10) 0.106(7) 0.034(6) 0.014(5) 0.007(6) C84 0.084(6) 0.165(9) 0.103(7) 0.029(6) 0.043(5) 0.018(6) C85 0.079(5) 0.104(5) 0.082(5) 0.006(4) 0.028(4) 0.031(4) C91 0.053(4) 0.069(4) 0.071(4) 0.003(3) -0.001(3) 0.003(3) C92 0.075(4) 0.068(5) 0.111(6) 0.026(4) -0.001(4) -0.010(4) C93 0.116(7) 0.117(7) 0.135(8) 0.074(6) -0.024(6) -0.037(5) C94 0.131(8) 0.208(11) 0.098(7) 0.076(7) -0.014(6) -0.065(8) C95 0.108(6) 0.165(8) 0.079(6) 0.035(5) -0.007(5) -0.017(6) C101 0.078(4) 0.062(4) 0.054(4) 0.001(3) 0.003(3) -0.007(3) C102 0.092(5) 0.085(5) 0.062(4) -0.003(3) 0.006(4) -0.010(4) C103 0.106(5) 0.072(5) 0.090(5) 0.012(4) 0.028(4) -0.002(4) C104 0.214(9) 0.069(5) 0.080(6) -0.004(4) 0.051(6) -0.036(6) C105 0.228(10) 0.086(6) 0.072(5) -0.019(4) 0.052(6) -0.052(6) C111 0.072(4) 0.056(4) 0.080(5) -0.006(3) 0.006(4) 0.005(3) C112 0.083(5) 0.067(5) 0.117(6) -0.004(4) -0.009(4) 0.020(4) C113 0.085(5) 0.076(5) 0.122(7) -0.019(5) 0.005(5) 0.007(4) C114 0.090(5) 0.084(5) 0.106(6) -0.037(4) 0.016(5) 0.004(4) C115 0.094(5) 0.068(4) 0.077(5) -0.014(4) -0.002(4) 0.002(4) C121 0.076(4) 0.052(4) 0.061(4) -0.004(3) 0.001(3) 0.009(3) C122 0.053(4) 0.113(6) 0.083(5) -0.006(4) -0.001(4) -0.001(4) C123 0.068(5) 0.145(7) 0.123(7) -0.005(6) -0.022(5) 0.019(5) C124 0.073(5) 0.150(7) 0.105(7) -0.020(6) 0.009(5) 0.027(5) C125 0.090(6) 0.129(6) 0.074(5) -0.002(4) 0.022(5) -0.003(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 N9 2.104(4) . ? Ag1 N3 2.124(4) . ? Ag1 Ag5 2.7522(6) . ? Ag1 Ag2 2.9083(6) . ? Ag2 N6 2.106(4) . ? Ag2 N12 2.123(4) . ? Ag2 Ag3 2.7641(6) . ? Ag3 N66 2.152(5) . ? Ag3 N126 2.169(5) . ? Ag4 N76 2.182(5) . ? Ag4 N116 2.215(5) . ? Ag4 O4 2.549(3) . ? Ag5 N36 2.185(5) . ? Ag5 N96 2.193(5) . ? Ag6 N106 2.181(5) . ? Ag6 N26 2.220(5) . ? Ag6 O1 2.549(3) . ? Ag7 N86 2.160(5) . ? Ag7 N56 2.177(5) . ? Ag7 O3 2.517(3) . ? Ag8 N16 2.174(5) . ? Ag8 N46 2.220(5) . ? Ag8 O2 2.581(4) . ? P1 O1 1.471(4) . ? P1 N3 1.604(4) . ? P1 N1 1.649(4) . ? P1 N2 1.686(4) . ? P2 O2 1.469(4) . ? P2 N6 1.605(4) . ? P2 N5 1.649(4) . ? P2 N4 1.682(4) . ? P3 O3 1.479(3) . ? P3 N9 1.606(4) . ? P3 N7 1.660(4) . ? P3 N8 1.688(4) . ? P4 O4 1.494(4) . ? P4 N12 1.603(4) . ? P4 N10 1.649(4) . ? P4 N11 1.673(4) . ? N1 C11 1.406(6) . ? N1 H1A 0.8600 . ? N2 C21 1.389(7) . ? N2 H2 0.8600 . ? N3 C31 1.406(6) . ? N4 C41 1.385(6) . ? N4 H4A 0.8600 . ? N5 C51 1.399(7) . ? N5 H5 0.8600 . ? N6 C61 1.390(7) . ? N7 C71 1.376(6) . ? N7 H7 0.8600 . ? N8 C81 1.383(7) . ? N8 H8A 0.8600 . ? N9 C91 1.405(7) . ? N10 C101 1.395(6) . ? N10 H10 0.8600 . ? N11 C111 1.380(7) . ? N11 H11 0.8600 . ? N12 C121 1.399(6) . ? N16 C11 1.337(6) . ? N16 C15 1.347(7) . ? N26 C21 1.335(7) . ? N26 C25 1.380(8) . ? N36 C35 1.338(7) . ? N36 C31 1.350(6) . ? N46 C41 1.341(7) . ? N46 C45 1.357(7) . ? N56 C51 1.336(6) . ? N56 C55 1.362(7) . ? N66 C65 1.343(7) . ? N66 C61 1.370(7) . ? N76 C71 1.340(7) . ? N76 C75 1.348(7) . ? N86 C81 1.356(7) . ? N86 C85 1.368(7) . ? N96 C91 1.339(7) . ? N96 C95 1.347(8) . ? N106 C101 1.309(7) . ? N106 C105 1.375(8) . ? N116 C115 1.359(7) . ? N116 C111 1.350(7) . ? N126 C121 1.326(6) . ? N126 C125 1.357(8) . ? C11 C12 1.394(7) . ? C12 C13 1.371(8) . ? C12 H12 0.9300 . ? C13 C14 1.398(8) . ? C13 H13 0.9300 . ? C14 C15 1.332(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C21 C22 1.413(8) . ? C22 C23 1.362(10) . ? C22 H22 0.9300 . ? C23 C24 1.366(11) . ? C23 H23 0.9300 . ? C24 C25 1.373(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C31 C32 1.372(7) . ? C32 C33 1.374(9) . ? C32 H32 0.9300 . ? C33 C34 1.381(9) . ? C33 H33 0.9300 . ? C34 C35 1.362(9) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C41 C42 1.380(8) . ? C42 C43 1.375(9) . ? C42 H42 0.9300 . ? C43 C44 1.353(10) . ? C43 H43 0.9300 . ? C44 C45 1.352(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C51 C52 1.378(7) . ? C52 C53 1.361(8) . ? C52 H52 0.9300 . ? C53 C54 1.357(8) . ? C53 H53 0.9300 . ? C54 C55 1.354(8) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C61 C62 1.405(8) . ? C62 C63 1.367(8) . ? C62 H62 0.9300 . ? C63 C64 1.358(9) . ? C63 H63 0.9300 . ? C64 C65 1.402(9) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C71 C72 1.360(8) . ? C72 C73 1.357(8) . ? C72 H72 0.9300 . ? C73 C74 1.397(9) . ? C73 H73 0.9300 . ? C74 C75 1.370(9) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C81 C82 1.397(8) . ? C82 C83 1.392(10) . ? C82 H82 0.9300 . ? C83 C84 1.372(11) . ? C83 H83 0.9300 . ? C84 C85 1.340(9) . ? C84 H84 0.9300 . ? C85 H85 0.9300 . ? C91 C92 1.391(8) . ? C92 C93 1.384(10) . ? C92 H92 0.9300 . ? C93 C94 1.353(12) . ? C93 H93 0.9300 . ? C94 C95 1.405(11) . ? C94 H94 0.9300 . ? C95 H95 0.9300 . ? C101 C102 1.367(8) . ? C102 C103 1.378(8) . ? C102 H102 0.9300 . ? C103 C104 1.320(9) . ? C103 H103 0.9300 . ? C104 C105 1.323(9) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? C111 C112 1.410(8) . ? C112 C113 1.359(9) . ? C112 H112 0.9300 . ? C113 C114 1.382(9) . ? C113 H113 0.9300 . ? C114 C115 1.380(9) . ? C114 H114 0.9300 . ? C115 H115 0.9300 . ? C121 C122 1.387(8) . ? C122 C123 1.381(9) . ? C122 H122 0.9300 . ? C123 C124 1.355(10) . ? C123 H123 0.9300 . ? C124 C125 1.326(9) . ? C124 H124 0.9300 . ? C125 H125 0.9300 . ? 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 N9 Ag1 N3 164.00(16) . . ? N9 Ag1 Ag5 80.25(11) . . ? N3 Ag1 Ag5 84.28(11) . . ? N9 Ag1 Ag2 99.90(11) . . ? N3 Ag1 Ag2 94.89(11) . . ? Ag5 Ag1 Ag2 172.37(2) . . ? N6 Ag2 N12 163.44(16) . . ? N6 Ag2 Ag3 82.13(11) . . ? N12 Ag2 Ag3 81.40(11) . . ? N6 Ag2 Ag1 101.05(11) . . ? N12 Ag2 Ag1 95.36(11) . . ? Ag3 Ag2 Ag1 166.29(2) . . ? N66 Ag3 N126 162.44(19) . . ? N66 Ag3 Ag2 80.91(13) . . ? N126 Ag3 Ag2 81.56(13) . . ? N76 Ag4 N116 168.58(19) . . ? N76 Ag4 O4 99.69(15) . . ? N116 Ag4 O4 89.83(15) . . ? N36 Ag5 N96 161.18(19) . . ? N36 Ag5 Ag1 78.83(13) . . ? N96 Ag5 Ag1 82.89(14) . . ? N106 Ag6 N26 168.8(2) . . ? N106 Ag6 O1 99.20(16) . . ? N26 Ag6 O1 88.55(16) . . ? N86 Ag7 N56 159.37(19) . . ? N86 Ag7 O3 91.99(17) . . ? N56 Ag7 O3 102.05(15) . . ? N16 Ag8 N46 162.52(18) . . ? N16 Ag8 O2 100.82(15) . . ? N46 Ag8 O2 88.08(15) . . ? O1 P1 N3 113.3(2) . . ? O1 P1 N1 110.5(2) . . ? N3 P1 N1 109.0(2) . . ? O1 P1 N2 111.9(2) . . ? N3 P1 N2 109.1(2) . . ? N1 P1 N2 102.5(2) . . ? O2 P2 N6 112.3(2) . . ? O2 P2 N5 112.2(2) . . ? N6 P2 N5 106.4(2) . . ? O2 P2 N4 112.2(2) . . ? N6 P2 N4 109.9(2) . . ? N5 P2 N4 103.3(2) . . ? O3 P3 N9 113.2(2) . . ? O3 P3 N7 110.9(2) . . ? N9 P3 N7 107.5(2) . . ? O3 P3 N8 111.5(2) . . ? N9 P3 N8 109.8(2) . . ? N7 P3 N8 103.3(2) . . ? O4 P4 N12 115.1(2) . . ? O4 P4 N10 109.6(2) . . ? N12 P4 N10 107.9(2) . . ? O4 P4 N11 110.8(2) . . ? N12 P4 N11 109.4(2) . . ? N10 P4 N11 103.3(2) . . ? P1 O1 Ag6 96.08(17) . . ? P2 O2 Ag8 93.68(17) . . ? P3 O3 Ag7 96.95(17) . . ? P4 O4 Ag4 97.92(17) . . ? C11 N1 P1 126.9(4) . . ? C11 N1 H1A 116.6 . . ? P1 N1 H1A 116.6 . . ? C21 N2 P1 128.9(4) . . ? C21 N2 H2 115.6 . . ? P1 N2 H2 115.6 . . ? C31 N3 P1 124.2(3) . . ? C31 N3 Ag1 115.2(3) . . ? P1 N3 Ag1 120.5(2) . . ? C41 N4 P2 127.2(4) . . ? C41 N4 H4A 116.4 . . ? P2 N4 H4A 116.4 . . ? C51 N5 P2 128.5(4) . . ? C51 N5 H5 115.8 . . ? P2 N5 H5 115.8 . . ? C61 N6 P2 122.2(4) . . ? C61 N6 Ag2 117.5(3) . . ? P2 N6 Ag2 119.7(2) . . ? C71 N7 P3 128.3(4) . . ? C71 N7 H7 115.8 . . ? P3 N7 H7 115.8 . . ? C81 N8 P3 127.5(4) . . ? C81 N8 H8A 116.2 . . ? P3 N8 H8A 116.2 . . ? C91 N9 P3 121.5(4) . . ? C91 N9 Ag1 119.7(3) . . ? P3 N9 Ag1 118.7(2) . . ? C101 N10 P4 127.4(4) . . ? C101 N10 H10 116.3 . . ? P4 N10 H10 116.3 . . ? C111 N11 P4 128.1(4) . . ? C111 N11 H11 116.0 . . ? P4 N11 H11 116.0 . . ? C121 N12 P4 124.0(4) . . ? C121 N12 Ag2 115.8(3) . . ? P4 N12 Ag2 119.4(2) . . ? C11 N16 C15 116.7(5) . . ? C11 N16 Ag8 125.6(4) . . ? C15 N16 Ag8 117.7(4) . . ? C21 N26 C25 117.4(6) . . ? C21 N26 Ag6 129.7(4) . . ? C25 N26 Ag6 112.9(5) . . ? C35 N36 C31 117.5(6) . . ? C35 N36 Ag5 115.7(5) . . ? C31 N36 Ag5 126.7(4) . . ? C41 N46 C45 116.4(5) . . ? C41 N46 Ag8 130.1(4) . . ? C45 N46 Ag8 113.3(4) . . ? C51 N56 C55 118.5(5) . . ? C51 N56 Ag7 124.3(4) . . ? C55 N56 Ag7 116.9(4) . . ? C65 N66 C61 118.9(5) . . ? C65 N66 Ag3 118.2(5) . . ? C61 N66 Ag3 123.0(4) . . ? C71 N76 C75 119.1(5) . . ? C71 N76 Ag4 125.3(4) . . ? C75 N76 Ag4 115.4(4) . . ? C81 N86 C85 116.9(6) . . ? C81 N86 Ag7 128.7(4) . . ? C85 N86 Ag7 114.1(5) . . ? C91 N96 C95 118.7(6) . . ? C91 N96 Ag5 121.1(4) . . ? C95 N96 Ag5 120.2(5) . . ? C101 N106 C105 117.0(6) . . ? C101 N106 Ag6 127.7(4) . . ? C105 N106 Ag6 115.3(5) . . ? C115 N116 C111 117.9(5) . . ? C115 N116 Ag4 112.2(4) . . ? C111 N116 Ag4 129.3(4) . . ? C121 N126 C125 118.4(6) . . ? C121 N126 Ag3 122.2(4) . . ? C125 N126 Ag3 119.4(5) . . ? N16 C11 C12 122.8(5) . . ? N16 C11 N1 116.9(5) . . ? C12 C11 N1 120.3(5) . . ? C13 C12 C11 118.1(6) . . ? C13 C12 H12 121.0 . . ? C11 C12 H12 121.0 . . ? C12 C13 C14 119.3(6) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 118.1(6) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C14 C15 N16 124.9(6) . . ? C14 C15 H15 117.6 . . ? N16 C15 H15 117.6 . . ? N26 C21 N2 119.7(5) . . ? N26 C21 C22 121.0(6) . . ? N2 C21 C22 119.2(6) . . ? C23 C22 C21 120.7(8) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 118.4(8) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 C23 119.8(8) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 N26 122.5(7) . . ? C24 C25 H25 118.7 . . ? N26 C25 H25 118.7 . . ? N36 C31 C32 122.0(5) . . ? N36 C31 N3 115.7(5) . . ? C32 C31 N3 122.2(5) . . ? C31 C32 C33 119.3(6) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C32 C33 C34 118.8(7) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C35 C34 C33 118.7(7) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? N36 C35 C34 123.4(7) . . ? N36 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? N46 C41 C42 122.2(6) . . ? N46 C41 N4 119.9(5) . . ? C42 C41 N4 117.8(6) . . ? C41 C42 C43 118.4(7) . . ? C41 C42 H42 120.8 . . ? C43 C42 H42 120.8 . . ? C44 C43 C42 120.8(7) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C45 C44 C43 117.4(7) . . ? C45 C44 H44 121.3 . . ? C43 C44 H44 121.3 . . ? C44 C45 N46 124.8(7) . . ? C44 C45 H45 117.6 . . ? N46 C45 H45 117.6 . . ? N56 C51 C52 120.3(6) . . ? N56 C51 N5 115.5(5) . . ? C52 C51 N5 124.2(5) . . ? C51 C52 C53 119.8(6) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 120.5(6) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C55 C54 C53 118.0(6) . . ? C55 C54 H54 121.0 . . ? C53 C54 H54 121.0 . . ? C54 C55 N56 122.8(6) . . ? C54 C55 H55 118.6 . . ? N56 C55 H55 118.6 . . ? N66 C61 N6 117.7(5) . . ? N66 C61 C62 118.0(6) . . ? N6 C61 C62 124.4(5) . . ? C63 C62 C61 122.6(6) . . ? C63 C62 H62 118.7 . . ? C61 C62 H62 118.7 . . ? C64 C63 C62 118.7(7) . . ? C64 C63 H63 120.7 . . ? C62 C63 H63 120.7 . . ? C63 C64 C65 118.3(6) . . ? C63 C64 H64 120.9 . . ? C65 C64 H64 120.9 . . ? N66 C65 C64 123.4(6) . . ? N66 C65 H65 118.3 . . ? C64 C65 H65 118.3 . . ? N76 C71 C72 121.4(6) . . ? N76 C71 N7 116.0(5) . . ? C72 C71 N7 122.5(6) . . ? C73 C72 C71 120.5(7) . . ? C73 C72 H72 119.8 . . ? C71 C72 H72 119.8 . . ? C72 C73 C74 118.6(7) . . ? C72 C73 H73 120.7 . . ? C74 C73 H73 120.7 . . ? C75 C74 C73 118.7(7) . . ? C75 C74 H74 120.7 . . ? C73 C74 H74 120.7 . . ? C74 C75 N76 121.6(7) . . ? C74 C75 H75 119.2 . . ? N76 C75 H75 119.2 . . ? N86 C81 N8 119.8(5) . . ? N86 C81 C82 122.6(7) . . ? N8 C81 C82 117.6(7) . . ? C83 C82 C81 117.2(8) . . ? C83 C82 H82 121.4 . . ? C81 C82 H82 121.4 . . ? C82 C83 C84 120.5(8) . . ? C82 C83 H83 119.8 . . ? C84 C83 H83 119.8 . . ? C85 C84 C83 119.1(8) . . ? C85 C84 H84 120.5 . . ? C83 C84 H84 120.5 . . ? C84 C85 N86 123.7(8) . . ? C84 C85 H85 118.2 . . ? N86 C85 H85 118.2 . . ? N96 C91 C92 121.1(6) . . ? N96 C91 N9 116.6(5) . . ? C92 C91 N9 122.3(6) . . ? C91 C92 C93 119.8(8) . . ? C91 C92 H92 120.1 . . ? C93 C92 H92 120.1 . . ? C94 C93 C92 119.0(8) . . ? C94 C93 H93 120.5 . . ? C92 C93 H93 120.5 . . ? C93 C94 C95 119.2(8) . . ? C93 C94 H94 120.4 . . ? C95 C94 H94 120.4 . . ? N96 C95 C94 121.8(8) . . ? N96 C95 H95 119.1 . . ? C94 C95 H95 119.1 . . ? N106 C101 C102 121.0(6) . . ? N106 C101 N10 117.1(5) . . ? C102 C101 N10 121.9(5) . . ? C101 C102 C103 120.3(6) . . ? C101 C102 H102 119.8 . . ? C103 C102 H102 119.8 . . ? C104 C103 C102 118.3(7) . . ? C104 C103 H103 120.9 . . ? C102 C103 H103 120.9 . . ? C105 C104 C103 120.2(7) . . ? C105 C104 H104 119.9 . . ? C103 C104 H104 119.9 . . ? C104 C105 N106 123.1(7) . . ? C104 C105 H105 118.4 . . ? N106 C105 H105 118.4 . . ? N116 C111 N11 119.3(5) . . ? N116 C111 C112 121.4(6) . . ? N11 C111 C112 119.3(6) . . ? C113 C112 C111 119.6(7) . . ? C113 C112 H112 120.2 . . ? C111 C112 H112 120.2 . . ? C112 C113 C114 119.4(7) . . ? C112 C113 H113 120.3 . . ? C114 C113 H113 120.3 . . ? C115 C114 C113 119.1(7) . . ? C115 C114 H114 120.5 . . ? C113 C114 H114 120.5 . . ? N116 C115 C114 122.5(6) . . ? N116 C115 H115 118.8 . . ? C114 C115 H115 118.8 . . ? N126 C121 C122 121.3(6) . . ? N126 C121 N12 118.9(5) . . ? C122 C121 N12 119.7(6) . . ? C121 C122 C123 117.2(6) . . ? C121 C122 H122 121.4 . . ? C123 C122 H122 121.4 . . ? C124 C123 C122 121.6(7) . . ? C124 C123 H123 119.2 . . ? C122 C123 H123 119.2 . . ? C125 C124 C123 117.6(7) . . ? C125 C124 H124 121.2 . . ? C123 C124 H124 121.2 . . ? C124 C125 N126 123.8(7) . . ? C124 C125 H125 118.1 . . ? N126 C125 H125 118.1 . . ? 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 N1 H1A O2 0.86 1.98 2.821(6) 163.9 . N5 H5 O3 0.86 1.95 2.804(5) 172.0 . N7 H7 O4 0.86 1.96 2.811(5) 171.1 . N10 H10 O1 0.86 1.97 2.827(5) 171.7 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.554 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.076