# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Robin D. Rogers' _publ_contact_author_address ;Department of Chemistry 313D Shelby Hall 500 Campus Drive The University of Alabama Tuscaloosa, AL 35487 ; _publ_contact_author_email rdrogers@ua.edu _publ_contact_author_phone '(205) 348-4323' _publ_contact_author_fax '(205) 348-0823' loop_ _publ_author_name _publ_author_address J.D.Holbery '' K.B.Vigour '' T.D.Morgan '' G.A.Broker '' R.D.Rogers ;Department of Chemistry 313D Shelby Hall 500 Campus Drive The University of Alabama Tuscaloosa, AL 35487 ; _publ_section_title ; Approaches to crystallization from ionic liquids: complex solvents-complex results or a strategy for controlled formation of new supramolecular architectures? ; data_1 _database_code_depnum_ccdc_archive 'CCDC 611317' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co(OH2)2(bipy)2)(NTf2)2(C4mim)(NTf2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H35 Co F18 N9 O14 S6' _chemical_formula_weight 1387.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 25.113(4) _cell_length_b 16.946(3) _cell_length_c 15.330(3) _cell_angle_alpha 90.00 _cell_angle_beta 126.371(3) _cell_angle_gamma 90.00 _cell_volume 5253.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 897 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 27.55 _exptl_crystal_description Rectangular _exptl_crystal_colour Pink _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2796 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.7401 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11791 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 23.30 _reflns_number_total 5253 _reflns_number_gt 4432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+5.0119P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 5253 _refine_ls_number_parameters 789 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 Co1 Co 0.19486(4) 0.25003(5) 0.38476(6) 0.0171(2) Uani 1 1 d . . . N1 N 0.1979(3) 0.1590(3) 0.2882(4) 0.0197(14) Uani 1 1 d . . . N2 N 0.1904(3) -0.1596(3) -0.0184(4) 0.0186(13) Uani 1 1 d . . . N3 N 0.1949(3) 0.3426(3) 0.4818(4) 0.0183(13) Uani 1 1 d . . . N4 N 0.1932(3) 0.6585(3) 0.7834(4) 0.0206(14) Uani 1 1 d . . . N5 N 0.4116(3) 0.4163(4) 0.5394(5) 0.0365(17) Uani 1 1 d . . . N6 N -0.0722(4) 0.3679(4) 0.1282(6) 0.052(2) Uani 1 1 d . . . N7 N 0.2207(4) 0.2481(5) 0.9019(7) 0.055(2) Uani 1 1 d . . . N25 N 0.5038(4) 0.2274(4) 1.0624(6) 0.0438(18) Uani 1 1 d . . . N26 N 0.4541(4) 0.3027(4) 0.9230(6) 0.0368(17) Uani 1 1 d . . . S1 S 0.45327(11) 0.44449(12) 0.66005(16) 0.0369(5) Uani 1 1 d . . . S2 S 0.43365(10) 0.35287(12) 0.49111(16) 0.0327(5) Uani 1 1 d . . . S3 S -0.07870(11) 0.36715(13) 0.21919(17) 0.0408(5) Uani 1 1 d . . . S4 S -0.01390(11) 0.40837(13) 0.13169(17) 0.0414(5) Uani 1 1 d . . . S5 S 0.23884(11) 0.29994(12) 0.84115(17) 0.0387(5) Uani 1 1 d . A . S6A S 0.2702(2) 0.16955(19) 0.9689(3) 0.0426(9) Uani 0.60 1 d P A 1 O11A O 0.3329(6) 0.1661(6) 0.9899(10) 0.059(3) Uani 0.60 1 d P A 1 F16A F 0.3172(8) 0.1332(6) 1.1640(8) 0.106(5) Uani 0.60 1 d P A 1 F17A F 0.3201(6) 0.2583(6) 1.1393(9) 0.082(3) Uani 0.60 1 d P A 1 F18A F 0.2338(7) 0.2004(7) 1.0933(10) 0.092(4) Uani 0.60 1 d P A 1 S6B S 0.2254(4) 0.1740(3) 0.9496(6) 0.0580(17) Uani 0.40 1 d P A 2 O11B O 0.1727(12) 0.1573(11) 0.9607(19) 0.090(7) Uani 0.40 1 d P A 2 F16B F 0.3076(16) 0.1164(17) 1.146(3) 0.185(14) Uani 0.40 1 d P A 2 F17B F 0.2894(13) 0.2451(11) 1.1366(16) 0.111(8) Uani 0.40 1 d P A 2 F18B F 0.3521(10) 0.1926(15) 1.0973(18) 0.126(8) Uani 0.40 1 d P A 2 O1 O 0.2983(2) 0.2508(3) 0.4845(4) 0.0245(12) Uani 1 1 d . . . O2 O 0.0904(3) 0.2431(3) 0.2834(4) 0.0250(12) Uani 1 1 d . . . O3 O 0.4093(3) 0.4796(3) 0.6775(5) 0.0451(15) Uani 1 1 d . . . O4 O 0.5014(3) 0.3901(3) 0.7388(4) 0.0394(14) Uani 1 1 d . . . O5 O 0.5002(3) 0.3258(3) 0.5615(4) 0.0384(14) Uani 1 1 d . . . O6 O 0.3830(3) 0.2953(3) 0.4316(4) 0.0409(14) Uani 1 1 d . . . O7 O -0.0198(3) 0.3674(5) 0.3296(6) 0.070(2) Uani 1 1 d . . . O8 O -0.1279(3) 0.3088(3) 0.1930(5) 0.0451(15) Uani 1 1 d . . . O9 O 0.0199(3) 0.4704(3) 0.2066(6) 0.0535(17) Uani 1 1 d . . . O10 O 0.0223(3) 0.3495(3) 0.1176(5) 0.0500(16) Uani 1 1 d . . . O11 O 0.1808(4) 0.3342(4) 0.7523(6) 0.088(3) Uani 1 1 d . . . O12 O 0.2815(5) 0.2665(5) 0.8200(8) 0.097(3) Uani 1 1 d . . . O13 O 0.2330(6) 0.1062(5) 0.9241(9) 0.131(4) Uani 1 1 d . . . F1 F 0.5326(3) 0.5616(3) 0.7657(4) 0.0630(15) Uani 1 1 d . . . F2 F 0.5509(3) 0.5027(3) 0.6627(5) 0.0557(14) Uani 1 1 d . . . F3 F 0.4674(3) 0.5798(3) 0.5936(4) 0.0588(14) Uani 1 1 d . . . F4 F 0.4406(3) 0.3627(3) 0.3300(5) 0.0651(17) Uani 1 1 d . . . F5 F 0.3716(2) 0.4445(3) 0.3202(4) 0.0569(14) Uani 1 1 d . . . F6 F 0.4761(3) 0.4657(3) 0.4298(4) 0.0554(14) Uani 1 1 d . . . F7 F -0.1766(3) 0.4669(3) 0.1036(5) 0.0683(16) Uani 1 1 d . . . F8 F -0.1395(3) 0.4602(4) 0.2695(5) 0.0711(18) Uani 1 1 d . . . F9 F -0.0819(3) 0.5207(3) 0.2305(6) 0.087(2) Uani 1 1 d . . . F10 F -0.1026(3) 0.5120(3) -0.0066(5) 0.0623(15) Uani 1 1 d . . . F11 F -0.0960(3) 0.4055(4) -0.0805(4) 0.0647(16) Uani 1 1 d . . . F12 F -0.0175(3) 0.4937(4) -0.0107(6) 0.088(2) Uani 1 1 d . . . F13 F 0.2498(4) 0.4174(4) 0.9572(7) 0.106(3) Uani 1 1 d . A . F14 F 0.2993(3) 0.4340(3) 0.8861(5) 0.0674(17) Uani 1 1 d . A . F15 F 0.3404(3) 0.3575(4) 1.0200(5) 0.091(2) Uani 1 1 d . A . C2 C 0.2435(4) 0.0998(4) 0.3364(6) 0.0253(17) Uani 1 1 d . . . H2A H 0.2779 0.1029 0.4119 0.030 Uiso 1 1 calc R . . C3 C 0.2413(4) 0.0355(4) 0.2790(6) 0.0235(16) Uani 1 1 d . . . H3A H 0.2738 -0.0048 0.3151 0.028 Uiso 1 1 calc R . . C4 C 0.1915(3) 0.0297(4) 0.1685(5) 0.0194(16) Uani 1 1 d . . . C5 C 0.1464(4) 0.0902(4) 0.1221(6) 0.0239(16) Uani 1 1 d . . . H5A H 0.1114 0.0885 0.0468 0.029 Uiso 1 1 calc R . . C6 C 0.1510(4) 0.1536(4) 0.1830(6) 0.0221(16) Uani 1 1 d . . . H6A H 0.1192 0.1948 0.1479 0.027 Uiso 1 1 calc R . . C7 C 0.1888(4) -0.0381(4) 0.1037(6) 0.0208(16) Uani 1 1 d . . . C8 C 0.2165(4) -0.1111(4) 0.1498(6) 0.0226(16) Uani 1 1 d . . . H8A H 0.2355 -0.1208 0.2239 0.027 Uiso 1 1 calc R . . C9 C 0.2160(4) -0.1695(4) 0.0866(6) 0.0279(18) Uani 1 1 d . . . H9A H 0.2347 -0.2193 0.1190 0.034 Uiso 1 1 calc R . . C12 C 0.1607(4) -0.0286(4) -0.0055(6) 0.0236(17) Uani 1 1 d . . . H12A H 0.1404 0.0200 -0.0409 0.028 Uiso 1 1 calc R . . C11 C 0.1625(4) -0.0900(4) -0.0617(6) 0.0241(16) Uani 1 1 d . . . H11A H 0.1425 -0.0825 -0.1366 0.029 Uiso 1 1 calc R . . C14 C 0.1406(4) 0.3577(4) 0.4774(6) 0.0262(17) Uani 1 1 d . . . H14A H 0.1031 0.3242 0.4357 0.031 Uiso 1 1 calc R . . C15 C 0.1382(4) 0.4215(4) 0.5329(6) 0.0249(17) Uani 1 1 d . . . H15A H 0.0990 0.4310 0.5272 0.030 Uiso 1 1 calc R . . C16 C 0.1916(4) 0.4707(4) 0.5954(5) 0.0187(16) Uani 1 1 d . . . C17 C 0.2470(4) 0.4541(4) 0.5988(6) 0.0279(17) Uani 1 1 d . . . H17A H 0.2852 0.4864 0.6408 0.033 Uiso 1 1 calc R . . C18 C 0.2469(4) 0.3911(4) 0.5417(6) 0.0230(16) Uani 1 1 d . . . H18A H 0.2853 0.3817 0.5448 0.028 Uiso 1 1 calc R . . C19 C 0.1910(4) 0.5377(4) 0.6577(6) 0.0217(17) Uani 1 1 d . . . C21 C 0.1613(4) 0.5909(4) 0.7658(6) 0.0235(16) Uani 1 1 d . . . H21A H 0.1384 0.5848 0.7974 0.028 Uiso 1 1 calc R . . C20 C 0.1589(4) 0.5298(5) 0.7062(6) 0.0277(18) Uani 1 1 d . . . H20A H 0.130(4) 0.479(5) 0.694(7) 0.05(2) Uiso 1 1 d . . . C24 C 0.2246(4) 0.6063(4) 0.6747(6) 0.0245(17) Uani 1 1 d . . . H24A H 0.255(3) 0.617(4) 0.652(5) 0.013(16) Uiso 1 1 d . . . C23 C 0.2250(4) 0.6658(4) 0.7390(6) 0.0222(16) Uani 1 1 d . . . H23A H 0.2490 0.7129 0.7512 0.027 Uiso 1 1 calc R . . C26 C 0.4456(5) 0.2511(5) 0.9770(7) 0.039(2) Uani 1 1 d . . . H26A H 0.4040 0.2335 0.9579 0.046 Uiso 1 1 calc R . . C28 C 0.5208(5) 0.3131(6) 0.9750(8) 0.047(2) Uani 1 1 d . . . H28A H 0.5413 0.3470 0.9537 0.057 Uiso 1 1 calc R . . C29 C 0.5500(5) 0.2670(6) 1.0595(9) 0.057(3) Uani 1 1 d . . . H29A H 0.5965 0.2617 1.1113 0.068 Uiso 1 1 calc R . . C30 C 0.4015(5) 0.3453(5) 0.8243(7) 0.048(2) Uani 1 1 d . . . H30A H 0.3582 0.3259 0.8011 0.072 Uiso 1 1 calc R . . H30B H 0.4066 0.3363 0.7664 0.072 Uiso 1 1 calc R . . H30C H 0.4049 0.4019 0.8398 0.072 Uiso 1 1 calc R . . C31 C 0.5156(6) 0.1736(6) 1.1469(7) 0.059(3) Uani 1 1 d . . . H31A H 0.5527 0.1378 1.1681 0.071 Uiso 1 1 calc R . . H31B H 0.4757 0.1409 1.1177 0.071 Uiso 1 1 calc R . . C32 C 0.5322(5) 0.2184(6) 1.2472(7) 0.054(2) Uani 1 1 d . . . H32A H 0.5691 0.2555 1.2718 0.064 Uiso 1 1 calc R . . H32B H 0.4933 0.2496 1.2279 0.064 Uiso 1 1 calc R . . C33 C 0.5518(6) 0.1615(6) 1.3391(8) 0.066(3) Uani 1 1 d . . . H33A H 0.5155 0.1232 1.3129 0.079 Uiso 1 1 calc R . . H33B H 0.5915 0.1316 1.3593 0.079 Uiso 1 1 calc R . . C34 C 0.5659(7) 0.2015(8) 1.4359(10) 0.093(4) Uani 1 1 d . . . H34A H 0.5722 0.1620 1.4879 0.139 Uiso 1 1 calc R . . H34B H 0.5287 0.2359 1.4152 0.139 Uiso 1 1 calc R . . H34C H 0.6062 0.2332 1.4691 0.139 Uiso 1 1 calc R . . C35 C 0.5039(4) 0.5267(5) 0.6695(7) 0.040(2) Uani 1 1 d . . . C36 C 0.4297(4) 0.4090(5) 0.3853(7) 0.035(2) Uani 1 1 d . . . C37 C -0.1210(5) 0.4586(6) 0.2092(9) 0.063(3) Uani 1 1 d . . . C38 C -0.0605(6) 0.4582(6) 0.0033(9) 0.061(3) Uiso 1 1 d . . . C39 C 0.2842(5) 0.3811(5) 0.9314(7) 0.044(2) Uani 1 1 d . . . C40 C 0.2914(6) 0.1889(6) 1.0971(10) 0.069(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0240(5) 0.0110(4) 0.0188(5) 0.0002(4) 0.0141(4) 0.0003(4) N1 0.019(3) 0.021(3) 0.019(3) -0.005(3) 0.011(3) -0.005(3) N2 0.032(3) 0.011(3) 0.015(3) 0.003(2) 0.016(3) 0.003(3) N3 0.029(3) 0.012(3) 0.022(3) 0.002(3) 0.019(3) 0.000(3) N4 0.023(3) 0.021(3) 0.015(3) 0.001(3) 0.010(3) 0.006(3) N5 0.030(4) 0.032(4) 0.040(4) 0.009(3) 0.016(3) 0.012(3) N6 0.050(5) 0.052(5) 0.061(5) -0.021(4) 0.037(5) -0.027(4) N7 0.055(5) 0.050(5) 0.063(5) 0.008(4) 0.037(5) -0.013(4) N25 0.053(5) 0.038(4) 0.043(5) 0.006(3) 0.030(4) 0.007(4) N26 0.049(5) 0.032(4) 0.043(4) 0.002(3) 0.034(4) 0.001(3) S1 0.0372(12) 0.0378(11) 0.0376(13) 0.0073(10) 0.0233(11) 0.0029(10) S2 0.0328(12) 0.0320(11) 0.0333(12) 0.0087(9) 0.0196(10) 0.0029(10) S3 0.0339(12) 0.0356(12) 0.0341(12) -0.0049(9) 0.0098(10) -0.0039(10) S4 0.0405(13) 0.0372(12) 0.0468(14) 0.0019(10) 0.0261(12) 0.0031(10) S5 0.0451(13) 0.0304(11) 0.0392(13) -0.0019(10) 0.0243(11) -0.0059(10) S6A 0.067(3) 0.0206(17) 0.063(2) 0.0084(17) 0.051(2) 0.0056(18) O11A 0.081(8) 0.054(6) 0.091(9) 0.033(6) 0.077(8) 0.035(6) F16A 0.214(15) 0.048(6) 0.070(7) 0.042(5) 0.092(9) 0.087(8) F17A 0.108(9) 0.069(7) 0.064(7) -0.011(5) 0.048(7) -0.022(7) F18A 0.121(10) 0.102(9) 0.116(10) -0.010(7) 0.104(9) -0.015(8) S6B 0.091(5) 0.034(3) 0.062(4) 0.001(3) 0.052(4) -0.007(3) O11B 0.119(18) 0.051(11) 0.132(18) 0.021(11) 0.092(17) -0.018(12) F16B 0.21(3) 0.16(2) 0.29(4) 0.12(3) 0.21(3) 0.04(2) F17B 0.20(3) 0.079(12) 0.090(14) 0.011(10) 0.105(17) 0.038(14) F18B 0.067(12) 0.17(2) 0.115(16) 0.057(15) 0.037(12) 0.037(14) O1 0.026(3) 0.023(3) 0.025(3) -0.002(2) 0.016(3) 0.001(2) O2 0.028(3) 0.024(3) 0.031(3) -0.009(2) 0.022(3) -0.005(2) O3 0.051(4) 0.047(3) 0.049(4) 0.003(3) 0.036(3) 0.010(3) O4 0.043(3) 0.035(3) 0.033(3) 0.009(3) 0.018(3) 0.007(3) O5 0.031(3) 0.039(3) 0.041(3) 0.017(3) 0.019(3) 0.017(3) O6 0.040(3) 0.037(3) 0.048(4) -0.003(3) 0.027(3) -0.013(3) O7 0.047(4) 0.087(5) 0.055(4) 0.001(4) 0.019(4) -0.015(4) O8 0.048(4) 0.037(3) 0.040(3) -0.003(3) 0.021(3) -0.008(3) O9 0.045(4) 0.041(3) 0.084(5) -0.037(3) 0.043(4) -0.022(3) O10 0.057(4) 0.037(3) 0.077(5) 0.009(3) 0.051(4) 0.018(3) O11 0.082(6) 0.061(4) 0.046(4) 0.014(4) -0.003(4) -0.030(4) O12 0.109(7) 0.074(5) 0.161(9) -0.066(6) 0.108(7) -0.039(5) O13 0.132(9) 0.054(5) 0.149(9) -0.051(6) 0.051(8) -0.011(6) F1 0.069(4) 0.056(3) 0.059(4) -0.012(3) 0.035(3) -0.008(3) F2 0.047(3) 0.053(3) 0.080(4) -0.002(3) 0.044(3) -0.006(3) F3 0.058(3) 0.042(3) 0.063(4) 0.026(3) 0.029(3) 0.012(3) F4 0.098(5) 0.061(3) 0.062(4) 0.008(3) 0.061(4) 0.008(3) F5 0.037(3) 0.074(4) 0.042(3) 0.033(3) 0.014(3) 0.009(3) F6 0.048(3) 0.051(3) 0.060(3) 0.018(3) 0.028(3) -0.010(3) F7 0.048(3) 0.068(4) 0.071(4) -0.003(3) 0.025(3) 0.013(3) F8 0.052(4) 0.098(5) 0.064(4) -0.044(3) 0.035(3) -0.018(3) F9 0.081(4) 0.049(3) 0.164(7) -0.061(4) 0.091(5) -0.033(3) F10 0.048(3) 0.054(3) 0.069(4) 0.012(3) 0.026(3) 0.019(3) F11 0.064(4) 0.081(4) 0.041(3) 0.014(3) 0.027(3) -0.002(3) F12 0.053(4) 0.108(5) 0.093(5) 0.048(4) 0.039(4) -0.006(4) F13 0.149(7) 0.074(4) 0.150(7) -0.056(5) 0.119(7) -0.027(5) F14 0.086(4) 0.040(3) 0.066(4) 0.000(3) 0.040(3) -0.025(3) F15 0.068(4) 0.062(4) 0.064(4) 0.003(3) -0.004(4) -0.024(4) C2 0.035(4) 0.016(4) 0.022(4) 0.000(3) 0.015(4) -0.005(3) C3 0.034(4) 0.019(4) 0.018(4) 0.002(3) 0.016(4) 0.003(3) C4 0.024(4) 0.014(4) 0.021(4) -0.003(3) 0.014(3) -0.008(3) C5 0.023(4) 0.023(4) 0.020(4) -0.001(3) 0.010(3) -0.003(3) C6 0.026(4) 0.015(3) 0.024(4) -0.005(3) 0.014(4) -0.003(3) C7 0.029(4) 0.017(4) 0.023(4) -0.002(3) 0.019(3) 0.002(3) C8 0.032(4) 0.021(4) 0.015(4) 0.000(3) 0.014(3) -0.003(3) C9 0.032(4) 0.017(4) 0.028(5) -0.005(3) 0.014(4) 0.002(3) C12 0.035(4) 0.015(4) 0.025(4) -0.001(3) 0.020(4) 0.005(3) C11 0.024(4) 0.024(4) 0.018(4) 0.006(3) 0.009(3) 0.007(3) C14 0.036(4) 0.015(4) 0.037(5) 0.002(3) 0.027(4) -0.001(3) C15 0.029(4) 0.024(4) 0.030(4) -0.002(3) 0.022(4) 0.004(3) C16 0.030(4) 0.017(4) 0.013(4) -0.003(3) 0.015(3) 0.003(3) C17 0.029(4) 0.019(4) 0.035(4) -0.004(3) 0.019(4) -0.005(3) C18 0.022(4) 0.018(4) 0.025(4) -0.004(3) 0.012(4) -0.001(3) C19 0.024(4) 0.012(4) 0.027(4) -0.001(3) 0.014(4) -0.003(3) C21 0.037(4) 0.018(4) 0.029(4) -0.003(3) 0.027(4) 0.000(3) C20 0.031(4) 0.026(4) 0.032(4) -0.004(4) 0.022(4) -0.003(4) C24 0.028(4) 0.022(4) 0.027(4) -0.001(3) 0.018(4) 0.009(3) C23 0.022(4) 0.018(3) 0.027(4) 0.005(3) 0.015(3) 0.004(3) C26 0.044(5) 0.028(4) 0.046(5) -0.004(4) 0.028(5) -0.001(4) C28 0.041(5) 0.051(5) 0.054(6) 0.001(5) 0.030(5) 0.003(5) C29 0.044(6) 0.059(6) 0.071(8) -0.005(6) 0.036(6) 0.005(5) C30 0.047(5) 0.039(5) 0.051(6) 0.003(4) 0.025(5) 0.000(4) C31 0.089(8) 0.042(5) 0.047(6) 0.009(5) 0.041(6) 0.009(6) C32 0.060(7) 0.047(5) 0.048(6) 0.003(5) 0.028(5) 0.002(5) C33 0.093(9) 0.059(6) 0.057(7) -0.002(5) 0.050(7) -0.015(6) C34 0.099(10) 0.095(10) 0.069(8) 0.009(7) 0.042(8) 0.012(9) C35 0.036(5) 0.038(5) 0.040(5) 0.009(4) 0.019(4) 0.010(4) C36 0.042(5) 0.033(4) 0.037(5) 0.011(4) 0.026(4) 0.000(4) C37 0.047(6) 0.059(7) 0.055(7) -0.030(5) 0.015(6) -0.007(5) C39 0.055(6) 0.050(5) 0.033(5) 0.002(4) 0.030(5) 0.001(5) C40 0.083(9) 0.041(6) 0.071(8) 0.018(6) 0.038(7) 0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.091(5) . ? Co1 O2 2.115(5) . ? Co1 N3 2.162(5) . ? Co1 N1 2.171(6) . ? Co1 N4 2.178(6) 2_564 ? Co1 N2 2.183(5) 2 ? N1 C6 1.321(9) . ? N1 C2 1.363(9) . ? N2 C11 1.329(9) . ? N2 C9 1.344(9) . ? N2 Co1 2.183(5) 2_554 ? N3 C18 1.343(9) . ? N3 C14 1.349(9) . ? N4 C23 1.328(9) . ? N4 C21 1.331(9) . ? N4 Co1 2.178(6) 2_565 ? N5 S1 1.565(7) . ? N5 S2 1.580(7) . ? N6 S3 1.497(8) . ? N6 S4 1.590(7) . ? N7 S6B 1.422(9) . ? N7 S5 1.534(7) . ? N7 S6A 1.691(9) . ? N25 C26 1.320(11) . ? N25 C29 1.364(12) . ? N25 C31 1.463(11) . ? N26 C26 1.306(10) . ? N26 C28 1.373(11) . ? N26 C30 1.479(11) . ? S1 O3 1.412(6) . ? S1 O4 1.428(6) . ? S1 C35 1.833(9) . ? S2 O6 1.423(6) . ? S2 O5 1.425(6) . ? S2 C36 1.831(7) . ? S3 O8 1.442(6) . ? S3 O7 1.444(7) . ? S3 C37 1.834(11) . ? S4 O9 1.410(6) . ? S4 O10 1.450(6) . ? S4 C38 1.795(11) . ? S5 O11 1.401(8) . ? S5 O12 1.409(8) . ? S5 C39 1.799(9) . ? S6A O13 1.318(10) . ? S6A O11A 1.407(12) . ? S6A C40 1.736(13) . ? F16A C40 1.254(13) . ? F17A C40 1.329(14) . ? F18A C40 1.426(16) . ? S6B O13 1.264(10) . ? S6B O11B 1.46(2) . ? S6B C40 1.865(14) . ? F16B C40 1.37(2) . ? F17B C40 1.146(18) . ? F18B C40 1.52(2) . ? F1 C35 1.335(10) . ? F2 C35 1.310(10) . ? F3 C35 1.319(9) . ? F4 C36 1.300(9) . ? F5 C36 1.326(10) . ? F6 C36 1.344(9) . ? F7 C37 1.382(11) . ? F8 C37 1.255(12) . ? F9 C37 1.341(12) . ? F10 C38 1.334(12) . ? F11 C38 1.373(12) . ? F12 C38 1.360(12) . ? F13 C39 1.298(11) . ? F14 C39 1.318(10) . ? F15 C39 1.313(11) . ? C2 C3 1.381(10) . ? C2 H2A 0.9500 . ? C3 C4 1.389(10) . ? C3 H3A 0.9500 . ? C4 C5 1.373(10) . ? C4 C7 1.494(9) . ? C5 C6 1.383(10) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.388(10) . ? C7 C8 1.390(10) . ? C8 C9 1.378(10) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C12 C11 1.370(10) . ? C12 H12A 0.9500 . ? C11 H11A 0.9500 . ? C14 C15 1.399(10) . ? C14 H14A 0.9500 . ? C15 C16 1.372(10) . ? C15 H15A 0.9500 . ? C16 C17 1.390(10) . ? C16 C19 1.489(9) . ? C17 C18 1.379(10) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.368(11) . ? C19 C20 1.389(10) . ? C21 C20 1.359(10) . ? C21 H21A 0.9500 . ? C20 H20A 1.07(9) . ? C24 C23 1.405(10) . ? C24 H24A 1.04(7) . ? C23 H23A 0.9500 . ? C26 H26A 0.9500 . ? C28 C29 1.305(13) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.535(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.528(13) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.470(15) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 Co1 O2 177.16(18) . . ? O1 Co1 N3 89.9(2) . . ? O2 Co1 N3 92.3(2) . . ? O1 Co1 N1 88.39(19) . . ? O2 Co1 N1 89.42(19) . . ? N3 Co1 N1 178.0(2) . . ? O1 Co1 N4 90.4(2) . 2_564 ? O2 Co1 N4 91.4(2) . 2_564 ? N3 Co1 N4 88.09(18) . 2_564 ? N1 Co1 N4 90.7(2) . 2_564 ? O1 Co1 N2 92.8(2) . 2 ? O2 Co1 N2 85.4(2) . 2 ? N3 Co1 N2 91.2(2) . 2 ? N1 Co1 N2 90.09(18) . 2 ? N4 Co1 N2 176.7(2) 2_564 2 ? C6 N1 C2 117.8(6) . . ? C6 N1 Co1 121.0(5) . . ? C2 N1 Co1 120.7(4) . . ? C11 N2 C9 116.5(6) . . ? C11 N2 Co1 120.4(4) . 2_554 ? C9 N2 Co1 123.1(4) . 2_554 ? C18 N3 C14 117.6(6) . . ? C18 N3 Co1 121.2(5) . . ? C14 N3 Co1 121.0(5) . . ? C23 N4 C21 116.7(6) . . ? C23 N4 Co1 122.5(5) . 2_565 ? C21 N4 Co1 120.8(4) . 2_565 ? S1 N5 S2 125.9(4) . . ? S3 N6 S4 125.4(5) . . ? S6B N7 S5 148.6(7) . . ? S6B N7 S6A 35.5(4) . . ? S5 N7 S6A 116.3(5) . . ? C26 N25 C29 106.3(8) . . ? C26 N25 C31 126.3(8) . . ? C29 N25 C31 127.3(9) . . ? C26 N26 C28 108.6(8) . . ? C26 N26 C30 126.4(8) . . ? C28 N26 C30 124.9(7) . . ? O3 S1 O4 118.5(3) . . ? O3 S1 N5 107.6(4) . . ? O4 S1 N5 116.1(3) . . ? O3 S1 C35 104.3(4) . . ? O4 S1 C35 102.9(4) . . ? N5 S1 C35 105.8(4) . . ? O6 S2 O5 117.8(4) . . ? O6 S2 N5 109.7(4) . . ? O5 S2 N5 116.4(4) . . ? O6 S2 C36 103.3(4) . . ? O5 S2 C36 105.2(4) . . ? N5 S2 C36 102.2(4) . . ? O8 S3 O7 116.2(4) . . ? O8 S3 N6 107.2(4) . . ? O7 S3 N6 119.4(4) . . ? O8 S3 C37 101.4(4) . . ? O7 S3 C37 103.6(5) . . ? N6 S3 C37 107.1(5) . . ? O9 S4 O10 120.4(4) . . ? O9 S4 N6 116.6(4) . . ? O10 S4 N6 110.2(4) . . ? O9 S4 C38 103.2(5) . . ? O10 S4 C38 102.7(4) . . ? N6 S4 C38 100.2(5) . . ? O11 S5 O12 116.0(6) . . ? O11 S5 N7 108.4(5) . . ? O12 S5 N7 116.8(5) . . ? O11 S5 C39 104.5(4) . . ? O12 S5 C39 105.2(5) . . ? N7 S5 C39 104.6(4) . . ? O13 S6A O11A 115.9(7) . . ? O13 S6A N7 106.6(6) . . ? O11A S6A N7 119.5(5) . . ? O13 S6A C40 113.0(7) . . ? O11A S6A C40 101.4(7) . . ? N7 S6A C40 99.2(5) . . ? O13 S6B N7 128.7(8) . . ? O13 S6B O11B 100.0(11) . . ? N7 S6B O11B 115.1(10) . . ? O13 S6B C40 108.1(8) . . ? N7 S6B C40 104.3(6) . . ? O11B S6B C40 95.8(10) . . ? S6B O13 S6A 44.7(4) . . ? N1 C2 C3 122.1(7) . . ? N1 C2 H2A 118.9 . . ? C3 C2 H2A 118.9 . . ? C2 C3 C4 119.9(7) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 116.7(6) . . ? C5 C4 C7 122.1(6) . . ? C3 C4 C7 121.2(6) . . ? C4 C5 C6 121.2(7) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? N1 C6 C5 122.3(7) . . ? N1 C6 H6A 118.9 . . ? C5 C6 H6A 118.9 . . ? C12 C7 C8 117.4(6) . . ? C12 C7 C4 120.2(6) . . ? C8 C7 C4 122.4(6) . . ? C9 C8 C7 119.2(6) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? N2 C9 C8 123.4(7) . . ? N2 C9 H9A 118.3 . . ? C8 C9 H9A 118.3 . . ? C11 C12 C7 119.2(6) . . ? C11 C12 H12A 120.4 . . ? C7 C12 H12A 120.4 . . ? N2 C11 C12 124.3(7) . . ? N2 C11 H11A 117.9 . . ? C12 C11 H11A 117.9 . . ? N3 C14 C15 121.4(7) . . ? N3 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C16 C15 C14 121.2(7) . . ? C16 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C15 C16 C17 116.4(6) . . ? C15 C16 C19 122.3(6) . . ? C17 C16 C19 121.3(6) . . ? C18 C17 C16 120.5(7) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? N3 C18 C17 122.8(7) . . ? N3 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C24 C19 C20 117.8(7) . . ? C24 C19 C16 122.1(6) . . ? C20 C19 C16 120.0(6) . . ? N4 C21 C20 124.9(6) . . ? N4 C21 H21A 117.6 . . ? C20 C21 H21A 117.6 . . ? C21 C20 C19 118.7(7) . . ? C21 C20 H20A 119(5) . . ? C19 C20 H20A 122(5) . . ? C19 C24 C23 119.4(7) . . ? C19 C24 H24A 126(3) . . ? C23 C24 H24A 114(3) . . ? N4 C23 C24 122.4(7) . . ? N4 C23 H23A 118.8 . . ? C24 C23 H23A 118.8 . . ? N26 C26 N25 109.4(8) . . ? N26 C26 H26A 125.3 . . ? N25 C26 H26A 125.3 . . ? C29 C28 N26 105.9(9) . . ? C29 C28 H28A 127.0 . . ? N26 C28 H28A 127.0 . . ? C28 C29 N25 109.8(9) . . ? C28 C29 H29A 125.1 . . ? N25 C29 H29A 125.1 . . ? N26 C30 H30A 109.5 . . ? N26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N25 C31 C32 111.7(8) . . ? N25 C31 H31A 109.3 . . ? C32 C31 H31A 109.3 . . ? N25 C31 H31B 109.3 . . ? C32 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? C33 C32 C31 111.1(8) . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 113.2(9) . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? F2 C35 F3 109.2(7) . . ? F2 C35 F1 107.7(7) . . ? F3 C35 F1 108.1(7) . . ? F2 C35 S1 111.9(6) . . ? F3 C35 S1 111.2(6) . . ? F1 C35 S1 108.6(6) . . ? F4 C36 F5 110.3(7) . . ? F4 C36 F6 107.8(7) . . ? F5 C36 F6 107.1(6) . . ? F4 C36 S2 110.1(5) . . ? F5 C36 S2 111.2(6) . . ? F6 C36 S2 110.3(6) . . ? F8 C37 F9 109.9(8) . . ? F8 C37 F7 107.7(9) . . ? F9 C37 F7 106.9(10) . . ? F8 C37 S3 113.9(8) . . ? F9 C37 S3 109.7(7) . . ? F7 C37 S3 108.5(6) . . ? F10 C38 F12 109.1(8) . . ? F10 C38 F11 107.9(9) . . ? F12 C38 F11 106.0(8) . . ? F10 C38 S4 113.8(7) . . ? F12 C38 S4 108.6(7) . . ? F11 C38 S4 111.1(7) . . ? F13 C39 F15 109.3(8) . . ? F13 C39 F14 106.8(8) . . ? F15 C39 F14 106.5(8) . . ? F13 C39 S5 111.3(7) . . ? F15 C39 S5 111.3(6) . . ? F14 C39 S5 111.4(6) . . ? F17B C40 F16A 110.8(14) . . ? F17B C40 F17A 35.8(13) . . ? F16A C40 F17A 113.6(12) . . ? F17B C40 F16B 123(2) . . ? F16A C40 F16B 15.5(17) . . ? F17A C40 F16B 129.0(19) . . ? F17B C40 F18A 63.0(15) . . ? F16A C40 F18A 99.0(11) . . ? F17A C40 F18A 98.2(11) . . ? F16B C40 F18A 96.4(13) . . ? F17B C40 F18B 108.9(19) . . ? F16A C40 F18B 90.0(11) . . ? F17A C40 F18B 73.2(12) . . ? F16B C40 F18B 93.7(16) . . ? F18A C40 F18B 169.6(13) . . ? F17B C40 S6A 132.5(12) . . ? F16A C40 S6A 116.5(9) . . ? F17A C40 S6A 115.6(9) . . ? F16B C40 S6A 103.9(17) . . ? F18A C40 S6A 110.9(9) . . ? F18B C40 S6A 69.2(10) . . ? F17B C40 S6B 117.9(14) . . ? F16A C40 S6B 123.1(9) . . ? F17A C40 S6B 123.0(8) . . ? F16B C40 S6B 107.6(18) . . ? F18A C40 S6B 79.5(8) . . ? F18B C40 S6B 100.2(11) . . ? S6A C40 S6B 31.4(3) . . ? 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 C37 S3 S4 C38 -49.2(5) . . . . ? C35 S1 S2 C36 -32.1(4) . . . . ? C39 S5 S6A C40 28.4(6) . . . . ? 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 C30 H30A O12 0.98 2.34 3.260(12) 156.8 . C26 H26A O11A 0.95 2.40 3.285(14) 154.2 . C6 H6A O5 0.95 2.47 3.092(9) 122.8 4_454 C29 H29A O11 0.95 2.52 3.309(13) 140.1 4 C26 H26A O12 0.95 2.56 3.328(14) 138.6 . C14 H14A O7 0.95 2.60 3.250(10) 126.0 . C30 H30B O8 0.98 2.63 3.106(11) 110.2 4 C20 H20A O11 1.07(9) 2.65(9) 3.366(11) 123(6) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.398 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.076 data_2 _database_code_depnum_ccdc_archive 'CCDC 611318' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Pd(pyriimdine)2)(OCOCH3)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 N4 O4 Pd' _chemical_formula_weight 384.67 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 8.523(2) _cell_length_b 7.595(2) _cell_length_c 10.564(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.224(5) _cell_angle_gamma 90.00 _cell_volume 683.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 851 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 23.30 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.869 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 1.379 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.6543 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1456 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0120 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 23.26 _reflns_number_total 938 _reflns_number_gt 891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.3084P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 938 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Pd1 Pd 0.5000 1.0000 0.5000 0.0173(2) Uani 1 2 d S . . N1 N 0.7148(2) 0.9096(3) 0.55402(19) 0.0196(5) Uani 1 1 d . . . N2 N 0.9201(3) 0.8957(3) 0.70841(19) 0.0271(5) Uani 1 1 d . . . O1 O 0.46909(19) 0.7897(2) 0.38860(15) 0.0219(4) Uani 1 1 d . . . O2 O 0.3204(2) 0.6534(3) 0.53023(17) 0.0311(5) Uani 1 1 d . . . C1 C 0.7793(3) 0.9456(5) 0.6686(3) 0.0231(6) Uani 1 1 d . . . H1 H 0.712(5) 1.008(3) 0.729(4) 0.019(11) Uiso 1 1 d . . . C2 C 1.0054(3) 0.8010(4) 0.6270(3) 0.0264(6) Uani 1 1 d . . . H2 H 1.110(4) 0.771(4) 0.651(3) 0.028(7) Uiso 1 1 d . . . C3 C 0.9484(4) 0.7556(4) 0.5091(3) 0.0251(6) Uani 1 1 d . . . H3 H 1.005(3) 0.695(4) 0.456(3) 0.014(7) Uiso 1 1 d . . . C4 C 0.8004(3) 0.8123(4) 0.4751(3) 0.0232(6) Uani 1 1 d . . . H4 H 0.753(3) 0.792(4) 0.406(3) 0.018(7) Uiso 1 1 d . . . C5 C 0.3781(3) 0.6630(3) 0.4255(2) 0.0192(6) Uani 1 1 d . . . C6 C 0.3491(5) 0.5260(5) 0.3244(4) 0.0263(9) Uani 1 1 d . . . H6C H 0.251(7) 0.485(4) 0.331(5) 0.034(14) Uiso 1 1 d . . . H6A H 0.418(5) 0.437(6) 0.342(4) 0.048(11) Uiso 1 1 d . . . H6B H 0.369(4) 0.577(5) 0.239(3) 0.037(8) 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 Pd1 0.0197(3) 0.0162(3) 0.0161(3) -0.00183(8) 0.00124(17) -0.00062(8) N1 0.0225(11) 0.0172(14) 0.0193(11) 0.0001(8) 0.0031(9) -0.0021(8) N2 0.0258(12) 0.0327(15) 0.0227(12) 0.0004(10) 0.0002(9) 0.0008(10) O1 0.0264(9) 0.0190(10) 0.0202(9) -0.0032(7) 0.0024(7) -0.0030(8) O2 0.0319(10) 0.0366(13) 0.0253(10) -0.0045(8) 0.0115(8) -0.0042(9) C1 0.0270(16) 0.0214(15) 0.0211(15) -0.0009(14) 0.0039(12) 0.0002(15) C2 0.0233(14) 0.0265(16) 0.0295(15) 0.0033(12) 0.0017(11) 0.0020(12) C3 0.0246(15) 0.0253(17) 0.0257(15) -0.0030(12) 0.0077(12) 0.0011(13) C4 0.0270(14) 0.0244(15) 0.0182(14) -0.0017(11) 0.0016(12) -0.0012(11) C5 0.0150(11) 0.0187(15) 0.0237(13) 0.0016(11) -0.0016(10) 0.0046(10) C6 0.025(2) 0.0229(18) 0.031(2) -0.0042(14) 0.0058(15) -0.0031(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O1 1.9977(17) . ? Pd1 O1 1.9977(17) 3_676 ? Pd1 N1 2.026(2) 3_676 ? Pd1 N1 2.026(2) . ? N1 C4 1.341(3) . ? N1 C1 1.346(4) . ? N2 C1 1.319(4) . ? N2 C2 1.346(4) . ? O1 C5 1.301(3) . ? O2 C5 1.222(3) . ? C1 H1 0.99(4) . ? C2 C3 1.371(4) . ? C2 H2 0.95(3) . ? C3 C4 1.373(4) . ? C3 H3 0.88(3) . ? C4 H4 0.84(3) . ? C5 C6 1.508(5) . ? C6 H6C 0.89(5) . ? C6 H6A 0.91(5) . ? C6 H6B 1.00(4) . ? 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 Pd1 O1 180.0 . 3_676 ? O1 Pd1 N1 89.87(7) . 3_676 ? O1 Pd1 N1 90.12(7) 3_676 3_676 ? O1 Pd1 N1 90.13(7) . . ? O1 Pd1 N1 89.88(7) 3_676 . ? N1 Pd1 N1 180.00(10) 3_676 . ? C4 N1 C1 117.0(2) . . ? C4 N1 Pd1 120.76(18) . . ? C1 N1 Pd1 122.22(18) . . ? C1 N2 C2 116.8(2) . . ? C5 O1 Pd1 119.12(15) . . ? N2 C1 N1 125.4(3) . . ? N2 C1 H1 118(3) . . ? N1 C1 H1 116(3) . . ? N2 C2 C3 121.9(3) . . ? N2 C2 H2 118.5(17) . . ? C3 C2 H2 119.5(17) . . ? C2 C3 C4 117.7(3) . . ? C2 C3 H3 121.5(19) . . ? C4 C3 H3 120.8(19) . . ? N1 C4 C3 121.2(3) . . ? N1 C4 H4 112.6(19) . . ? C3 C4 H4 126.2(19) . . ? O2 C5 O1 124.7(2) . . ? O2 C5 C6 122.5(3) . . ? O1 C5 C6 112.8(2) . . ? C5 C6 H6C 109(3) . . ? C5 C6 H6A 106(3) . . ? H6C C6 H6A 109(4) . . ? C5 C6 H6B 110(2) . . ? H6C C6 H6B 113(3) . . ? H6A C6 H6B 111(3) . . ? 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 C2 H2 O2 0.95(3) 2.39(3) 3.102(3) 131(2) 1_655 _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.528 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.097 data_3 _database_code_depnum_ccdc_archive 'CCDC 611319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ag(CH3CN)(bipy))(NTf2)*CH3CN _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H14 Ag F6 N5 O4 S2' _chemical_formula_weight 626.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 8.439(6) _cell_length_b 29.12(2) _cell_length_c 10.064(8) _cell_angle_alpha 90.00 _cell_angle_beta 113.611(12) _cell_angle_gamma 90.00 _cell_volume 2266(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 922 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 23.20 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 1.157 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.5028 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8289 _diffrn_reflns_av_R_equivalents 0.0985 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3170 _reflns_number_gt 2948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+0.8957P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3170 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 -0.24730(2) 0.742990(7) -0.14447(2) 0.02836(11) Uani 1 1 d . . . N1 N -0.0656(3) 0.74700(6) -0.2479(2) 0.0235(5) Uani 1 1 d . . . N2 N 0.5672(3) 0.75316(6) -0.5458(2) 0.0239(5) Uani 1 1 d . . . N3 N -0.2135(4) 0.65402(9) -0.1174(3) 0.0522(7) Uani 1 1 d . . . N4 N -0.5130(3) 0.88505(7) -0.2093(3) 0.0361(6) Uani 1 1 d . . . N5 N 0.3435(4) 0.61123(10) -0.2376(4) 0.0649(9) Uani 1 1 d . . . S1 S -0.65743(10) 0.92187(2) -0.28988(8) 0.0377(2) Uani 1 1 d . . . S2 S -0.31947(10) 0.88873(2) -0.18789(7) 0.03178(18) Uani 1 1 d . . . O1 O -0.7946(3) 0.90126(7) -0.4102(2) 0.0509(6) Uani 1 1 d . . . O2 O -0.5988(3) 0.96639(6) -0.3087(3) 0.0522(6) Uani 1 1 d . . . O3 O -0.2886(3) 0.91370(7) -0.2964(2) 0.0466(5) Uani 1 1 d . . . O4 O -0.2413(3) 0.84449(7) -0.1454(2) 0.0460(6) Uani 1 1 d . . . F1 F -0.0455(3) 0.92447(9) 0.0102(3) 0.0929(8) Uani 1 1 d . . . F2 F -0.2365(3) 0.90291(8) 0.0868(2) 0.0843(8) Uani 1 1 d . . . F3 F -0.2734(3) 0.96451(6) -0.0359(2) 0.0650(6) Uani 1 1 d . . . F4 F -0.6313(3) 0.94526(7) -0.0311(2) 0.0680(6) Uani 1 1 d . . . F5 F -0.8771(3) 0.95956(7) -0.2040(3) 0.0754(6) Uani 1 1 d . . . F6 F -0.8096(3) 0.89005(6) -0.1278(2) 0.0676(6) Uani 1 1 d . . . C2 C -0.0177(4) 0.70902(9) -0.2979(3) 0.0293(6) Uani 1 1 d . . . H2A H -0.073(4) 0.6811(10) -0.289(3) 0.044(8) Uiso 1 1 d . . . C3 C 0.1008(4) 0.70898(8) -0.3583(3) 0.0279(6) Uani 1 1 d . . . H3A H 0.125(4) 0.6835(10) -0.392(3) 0.039(8) Uiso 1 1 d . . . C4 C 0.1830(4) 0.74974(7) -0.3678(3) 0.0206(5) Uani 1 1 d . . . C5 C 0.1318(4) 0.78901(8) -0.3178(3) 0.0270(6) Uani 1 1 d . . . H5A H 0.182(4) 0.8180(9) -0.321(3) 0.036(8) Uiso 1 1 d . . . C6 C 0.0097(4) 0.78644(9) -0.2602(3) 0.0284(6) Uani 1 1 d . . . H6A H -0.026(3) 0.8117(9) -0.226(3) 0.028(7) Uiso 1 1 d . . . C7 C 0.3170(3) 0.75095(7) -0.4268(3) 0.0206(5) Uani 1 1 d . . . C8 C 0.4089(3) 0.71164(8) -0.4338(3) 0.0249(6) Uani 1 1 d . . . H8A H 0.390(4) 0.6830(10) -0.396(3) 0.039(8) Uiso 1 1 d . . . C9 C 0.3581(4) 0.79146(8) -0.4799(3) 0.0264(6) Uani 1 1 d . . . H9A H 0.302(4) 0.8205(9) -0.483(3) 0.037(8) Uiso 1 1 d . . . C10 C 0.5281(3) 0.71406(8) -0.4939(3) 0.0260(6) Uani 1 1 d . . . H10A H 0.589(4) 0.6890(9) -0.503(3) 0.030(7) Uiso 1 1 d . . . C11 C 0.4812(4) 0.79105(9) -0.5368(3) 0.0275(6) Uani 1 1 d . . . H11A H 0.508(4) 0.8165(9) -0.577(3) 0.030(7) Uiso 1 1 d . . . C13 C -0.2117(4) 0.61545(10) -0.1020(3) 0.0382(7) Uani 1 1 d . . . C14 C -0.2105(6) 0.56613(10) -0.0833(4) 0.0486(9) Uani 1 1 d . . . H14A H -0.100(7) 0.5557(15) -0.059(5) 0.097(16) Uiso 1 1 d . . . H14B H -0.276(5) 0.5520(13) -0.169(4) 0.070(12) Uiso 1 1 d . . . H14C H -0.256(7) 0.5593(15) -0.016(5) 0.099(16) Uiso 1 1 d . . . C15 C -0.7479(4) 0.92928(11) -0.1538(4) 0.0497(9) Uani 1 1 d . . . C16 C -0.2131(4) 0.92229(11) -0.0227(3) 0.0478(8) Uani 1 1 d . . . C17 C 0.3072(4) 0.57573(10) -0.2130(3) 0.0443(8) Uani 1 1 d . . . C18 C 0.2598(5) 0.53034(10) -0.1817(4) 0.0577(9) Uani 1 1 d . . . H18A H 0.1436 0.5226 -0.2526 0.087 Uiso 1 1 calc R . . H18B H 0.2609 0.5300 -0.0840 0.087 Uiso 1 1 calc R . . H18C H 0.3428 0.5077 -0.1875 0.087 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 0.02365(16) 0.04094(15) 0.02887(16) -0.00202(8) 0.01929(11) -0.00194(8) N1 0.0194(12) 0.0307(11) 0.0230(12) -0.0022(8) 0.0113(10) -0.0022(8) N2 0.0233(13) 0.0288(11) 0.0230(12) 0.0006(8) 0.0129(10) 0.0017(8) N3 0.0644(19) 0.0351(16) 0.079(2) 0.0059(13) 0.0514(17) 0.0019(12) N4 0.0394(15) 0.0236(10) 0.0525(15) 0.0086(10) 0.0259(12) 0.0054(9) N5 0.064(2) 0.0415(17) 0.080(2) 0.0009(15) 0.0186(18) -0.0063(13) S1 0.0371(4) 0.0255(3) 0.0507(5) 0.0041(3) 0.0178(4) 0.0027(3) S2 0.0390(4) 0.0277(3) 0.0381(4) 0.0030(3) 0.0254(4) 0.0033(3) O1 0.0448(13) 0.0458(12) 0.0553(14) -0.0006(10) 0.0130(11) -0.0026(9) O2 0.0498(14) 0.0287(10) 0.0727(15) 0.0155(10) 0.0188(12) 0.0044(9) O3 0.0581(14) 0.0478(11) 0.0479(12) 0.0035(9) 0.0359(11) -0.0054(10) O4 0.0504(14) 0.0329(11) 0.0711(15) 0.0089(9) 0.0414(12) 0.0146(8) F1 0.0409(14) 0.136(2) 0.0862(17) -0.0408(16) 0.0095(12) -0.0030(12) F2 0.132(2) 0.0873(15) 0.0379(11) 0.0082(11) 0.0386(13) 0.0211(14) F3 0.0788(15) 0.0429(10) 0.0612(12) -0.0168(9) 0.0152(11) 0.0005(9) F4 0.0729(15) 0.0681(12) 0.0687(14) -0.0203(11) 0.0345(12) 0.0076(10) F5 0.0573(13) 0.0600(12) 0.1134(18) -0.0070(12) 0.0391(13) 0.0259(10) F6 0.0770(15) 0.0524(11) 0.1033(16) -0.0031(11) 0.0674(13) -0.0013(10) C2 0.0303(16) 0.0290(14) 0.0371(16) -0.0033(11) 0.0223(13) -0.0059(11) C3 0.0304(16) 0.0251(13) 0.0365(15) -0.0059(11) 0.0220(13) -0.0022(11) C4 0.0185(15) 0.0262(13) 0.0168(13) 0.0006(9) 0.0067(11) 0.0013(9) C5 0.0308(16) 0.0233(13) 0.0352(15) 0.0005(10) 0.0221(13) -0.0010(11) C6 0.0291(16) 0.0285(13) 0.0340(15) -0.0024(11) 0.0193(13) 0.0026(11) C7 0.0182(14) 0.0275(12) 0.0178(13) -0.0022(9) 0.0089(11) -0.0010(9) C8 0.0246(15) 0.0240(13) 0.0317(14) -0.0009(10) 0.0170(12) -0.0017(10) C9 0.0306(16) 0.0246(13) 0.0307(14) 0.0026(10) 0.0194(13) 0.0031(11) C10 0.0273(15) 0.0255(13) 0.0311(15) -0.0033(11) 0.0177(12) 0.0016(11) C11 0.0302(16) 0.0278(13) 0.0312(15) 0.0069(11) 0.0193(13) 0.0019(11) C13 0.0434(19) 0.0368(18) 0.0469(18) -0.0011(13) 0.0313(15) -0.0018(13) C14 0.067(3) 0.0309(16) 0.056(2) -0.0018(15) 0.034(2) -0.0014(16) C15 0.045(2) 0.0393(17) 0.071(2) -0.0059(16) 0.0309(19) 0.0093(14) C16 0.046(2) 0.0536(19) 0.0398(19) -0.0008(15) 0.0131(16) 0.0102(15) C17 0.0441(19) 0.0357(17) 0.0459(18) -0.0045(14) 0.0104(15) 0.0057(14) C18 0.078(3) 0.0355(17) 0.063(2) 0.0000(15) 0.032(2) 0.0004(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.167(3) 4_476 ? Ag1 N1 2.174(3) . ? Ag1 N3 2.609(3) . ? N1 C6 1.342(3) . ? N1 C2 1.342(3) . ? N2 C11 1.344(3) . ? N2 C10 1.348(3) . ? N2 Ag1 2.167(3) 4_675 ? N3 C13 1.133(4) . ? N4 S2 1.563(3) . ? N4 S1 1.581(2) . ? N5 C17 1.133(4) . ? S1 O2 1.427(2) . ? S1 O1 1.429(2) . ? S1 C15 1.828(4) . ? S2 O3 1.420(2) . ? S2 O4 1.432(2) . ? S2 C16 1.825(3) . ? F1 C16 1.319(4) . ? F2 C16 1.321(4) . ? F3 C16 1.316(4) . ? F4 C15 1.318(4) . ? F5 C15 1.335(4) . ? F6 C15 1.324(4) . ? C2 C3 1.363(4) . ? C2 H2A 0.96(3) . ? C3 C4 1.397(4) . ? C3 H3A 0.87(3) . ? C4 C5 1.386(4) . ? C4 C7 1.473(4) . ? C5 C6 1.372(4) . ? C5 H5A 0.95(3) . ? C6 H6A 0.91(3) . ? C7 C9 1.395(4) . ? C7 C8 1.401(4) . ? C8 C10 1.366(4) . ? C8 H8A 0.96(3) . ? C9 C11 1.372(4) . ? C9 H9A 0.96(3) . ? C10 H10A 0.92(3) . ? C11 H11A 0.91(3) . ? C13 C14 1.448(4) . ? C14 H14A 0.92(5) . ? C14 H14B 0.92(4) . ? C14 H14C 0.93(5) . ? C17 C18 1.451(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 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 N2 Ag1 N1 173.84(7) 4_476 . ? N2 Ag1 N3 94.15(8) 4_476 . ? N1 Ag1 N3 92.00(8) . . ? C6 N1 C2 116.5(2) . . ? C6 N1 Ag1 122.75(17) . . ? C2 N1 Ag1 120.73(17) . . ? C11 N2 C10 116.4(2) . . ? C11 N2 Ag1 119.83(17) . 4_675 ? C10 N2 Ag1 123.75(17) . 4_675 ? C13 N3 Ag1 173.6(2) . . ? S2 N4 S1 124.90(14) . . ? O2 S1 O1 118.37(14) . . ? O2 S1 N4 116.56(14) . . ? O1 S1 N4 110.25(14) . . ? O2 S1 C15 105.26(15) . . ? O1 S1 C15 104.15(16) . . ? N4 S1 C15 99.37(14) . . ? O3 S2 O4 119.08(14) . . ? O3 S2 N4 115.62(13) . . ? O4 S2 N4 108.07(12) . . ? O3 S2 C16 104.58(15) . . ? O4 S2 C16 102.11(14) . . ? N4 S2 C16 105.50(15) . . ? N1 C2 C3 123.6(2) . . ? N1 C2 H2A 115.8(19) . . ? C3 C2 H2A 120.6(19) . . ? C2 C3 C4 120.2(2) . . ? C2 C3 H3A 120(2) . . ? C4 C3 H3A 119(2) . . ? C5 C4 C3 116.2(3) . . ? C5 C4 C7 121.8(2) . . ? C3 C4 C7 122.0(2) . . ? C6 C5 C4 120.3(2) . . ? C6 C5 H5A 118.9(18) . . ? C4 C5 H5A 120.8(18) . . ? N1 C6 C5 123.3(2) . . ? N1 C6 H6A 114.6(17) . . ? C5 C6 H6A 122.1(17) . . ? C9 C7 C8 116.3(2) . . ? C9 C7 C4 121.6(2) . . ? C8 C7 C4 122.1(2) . . ? C10 C8 C7 120.1(2) . . ? C10 C8 H8A 119.7(18) . . ? C7 C8 H8A 120.2(18) . . ? C11 C9 C7 119.9(2) . . ? C11 C9 H9A 116.0(18) . . ? C7 C9 H9A 124.0(18) . . ? N2 C10 C8 123.6(2) . . ? N2 C10 H10A 113.5(17) . . ? C8 C10 H10A 122.9(17) . . ? N2 C11 C9 123.7(2) . . ? N2 C11 H11A 113.9(18) . . ? C9 C11 H11A 122.4(18) . . ? N3 C13 C14 179.6(4) . . ? C13 C14 H14A 108(3) . . ? C13 C14 H14B 111(2) . . ? H14A C14 H14B 105(4) . . ? C13 C14 H14C 109(3) . . ? H14A C14 H14C 114(4) . . ? H14B C14 H14C 109(4) . . ? F4 C15 F6 108.9(3) . . ? F4 C15 F5 108.2(3) . . ? F6 C15 F5 108.6(3) . . ? F4 C15 S1 111.4(2) . . ? F6 C15 S1 111.2(2) . . ? F5 C15 S1 108.5(2) . . ? F3 C16 F1 108.2(3) . . ? F3 C16 F2 107.6(3) . . ? F1 C16 F2 108.4(3) . . ? F3 C16 S2 112.3(2) . . ? F1 C16 S2 109.9(2) . . ? F2 C16 S2 110.4(2) . . ? N5 C17 C18 179.7(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C14 H14C O3 0.93(5) 2.46(5) 3.263(5) 145(4) 4_576 C6 H6A O4 0.91(3) 2.46(3) 3.262(4) 147(2) . C18 H18B O2 0.98 2.54 3.455(5) 155.1 4_676 C18 H18C O2 0.98 2.49 3.448(5) 166.4 2_544 C10 H10A O4 0.92(3) 2.59(3) 3.376(4) 144(2) 4_675 C5 H5A O1 0.95(3) 2.62(3) 3.521(4) 158(2) 1_655 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.301 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.084 data_4 _database_code_depnum_ccdc_archive 'CCDC 611320' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ag(pyrimidine)2)3(BF4)(NTf2)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Ag3 B F16 N14 O8 S4' _chemical_formula_weight 1451.27 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 6.328(3) _cell_length_b 31.404(14) _cell_length_c 24.166(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4802(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 1.508 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20084 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 23.31 _reflns_number_total 3536 _reflns_number_gt 3266 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+65.0791P] 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 3536 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1473 _refine_ls_goodness_of_fit_ref 1.360 _refine_ls_restrained_S_all 1.360 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.19404(12) 0.39809(2) 0.61863(3) 0.0318(2) Uani 1 1 d . . . Ag2 Ag 1.18346(17) 0.22718(3) 0.7500 0.0324(3) Uani 1 2 d S . . B1 B 1.701(3) 0.3435(5) 0.7500 0.032(4) Uani 1 2 d S . . F1 F 1.4431(15) 0.2010(2) 0.5874(4) 0.086(3) Uani 1 1 d . . . F2 F 1.5903(12) 0.1421(3) 0.6089(4) 0.079(3) Uani 1 1 d . . . F3 F 1.4993(13) 0.1540(2) 0.5255(3) 0.068(2) Uani 1 1 d . . . F4 F 0.9113(11) 0.0605(2) 0.6687(4) 0.071(2) Uani 1 1 d . . . F5 F 0.9365(10) 0.0139(2) 0.6066(3) 0.0526(19) Uani 1 1 d . . . F6 F 1.0744(11) 0.0021(2) 0.6849(3) 0.0563(19) Uani 1 1 d . . . F7 F 1.888(2) 0.3300(5) 0.7500 0.163(9) Uani 1 2 d S A . F9 F 1.716(5) 0.3883(9) 0.7500 0.103(9) Uiso 0.50 2 d SP A 1 F10 F 1.629(5) 0.3355(9) 0.6990(13) 0.173(11) Uiso 0.50 1 d P A 1 F9A F 1.554(5) 0.3129(9) 0.7500 0.101(9) Uiso 0.50 2 d SP A 2 F10A F 1.665(6) 0.3708(12) 0.7120(14) 0.215(15) Uiso 0.50 1 d P A 2 S1 S 1.1867(5) 0.13745(8) 0.59266(11) 0.0347(6) Uani 1 1 d . . . S2 S 1.2834(4) 0.05473(8) 0.62545(10) 0.0265(6) Uani 1 1 d . . . O1 O 1.1465(12) 0.1492(2) 0.6482(3) 0.0412(19) Uani 1 1 d . . . O2 O 1.0566(14) 0.1544(2) 0.5507(3) 0.051(2) Uani 1 1 d . . . O3 O 1.3747(11) 0.0705(2) 0.6749(3) 0.042(2) Uani 1 1 d . . . O4 O 1.3814(11) 0.0203(2) 0.5969(3) 0.0410(19) Uani 1 1 d . . . N1 N 1.2186(14) 0.0883(3) 0.5811(3) 0.031(2) Uani 1 1 d . . . N2 N 1.2678(11) 0.4304(2) 0.7015(3) 0.0232(18) Uani 1 1 d . . . N4 N 0.5089(12) 0.4200(2) 0.5756(3) 0.026(2) Uani 1 1 d . . . N6 N 0.8805(12) 0.4178(3) 0.5743(4) 0.031(2) Uani 1 1 d . . . N8 N 1.1260(14) 0.3265(3) 0.6161(4) 0.036(2) Uani 1 1 d . . . N9 N 1.1085(14) 0.2629(2) 0.6689(4) 0.034(2) Uani 1 1 d . . . N10 N 0.8610(16) 0.1888(3) 0.7500 0.028(3) Uani 1 2 d S . . N12 N 0.4902(18) 0.1907(4) 0.7500 0.025(3) Uani 1 2 d S . . C1 C 1.450(2) 0.1597(4) 0.5774(5) 0.049(3) Uani 1 1 d . . . C2 C 1.0357(17) 0.0317(4) 0.6478(5) 0.038(3) Uani 1 1 d . . . C3 C 1.3883(15) 0.4654(3) 0.7022(4) 0.027(2) Uani 1 1 d . . . H3B H 1.4297 0.4778 0.6680 0.032 Uiso 1 1 calc R . . C4 C 1.453(2) 0.4839(4) 0.7500 0.029(3) Uani 1 2 d S . . H4C H 1.5405 0.5085 0.7500 0.035 Uiso 1 2 calc SR . . C7 C 1.214(2) 0.4149(5) 0.7500 0.031(3) Uani 1 2 d S . . H7A H 1.1275 0.3901 0.7500 0.037 Uiso 1 2 calc SR . . C9 C 0.5120(17) 0.4388(4) 0.5263(4) 0.036(3) Uani 1 1 d . . . H9A H 0.3821 0.4471 0.5098 0.043 Uiso 1 1 calc R . . C10 C 0.6953(16) 0.4464(4) 0.4987(4) 0.041(3) Uani 1 1 d . . . H10A H 0.6960 0.4590 0.4629 0.049 Uiso 1 1 calc R . . C14 C 0.6956(15) 0.4111(3) 0.5976(4) 0.030(2) Uani 1 1 d . . . H14A H 0.6958 0.3988 0.6335 0.036 Uiso 1 1 calc R . . C19 C 0.8789(15) 0.4350(4) 0.5247(4) 0.034(3) Uani 1 1 d . . . H19A H 1.0096 0.4398 0.5064 0.041 Uiso 1 1 calc R . . C21 C 1.1743(17) 0.3021(3) 0.6589(5) 0.036(3) Uani 1 1 d . . . H21A H 1.2671 0.3142 0.6855 0.044 Uiso 1 1 calc R . . C25 C 0.997(2) 0.3091(4) 0.5792(5) 0.048(3) Uani 1 1 d . . . H25A H 0.9590 0.3252 0.5474 0.058 Uiso 1 1 calc R . . C26 C 0.916(2) 0.2690(4) 0.5847(5) 0.057(4) Uani 1 1 d . . . H26A H 0.8223 0.2572 0.5580 0.069 Uiso 1 1 calc R . . C27 C 0.977(2) 0.2467(4) 0.6306(4) 0.044(3) Uani 1 1 d . . . H27A H 0.9236 0.2187 0.6356 0.053 Uiso 1 1 calc R . . C30 C 0.855(2) 0.1463(4) 0.7500 0.026(3) Uani 1 2 d S . . H30A H 0.9835 0.1307 0.7500 0.031 Uiso 1 2 calc SR . . C31 C 0.679(2) 0.2084(4) 0.7500 0.031(3) Uani 1 2 d S . . H31A H 0.6835 0.2387 0.7500 0.037 Uiso 1 2 calc SR . . C32 C 0.671(2) 0.1254(4) 0.7500 0.028(3) Uani 1 2 d S . . H32A H 0.6680 0.0951 0.7500 0.034 Uiso 1 2 calc SR . . C34 C 0.486(2) 0.1484(5) 0.7500 0.032(4) Uani 1 2 d S . . H34A H 0.3544 0.1340 0.7500 0.038 Uiso 1 2 calc SR . . 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 0.0223(4) 0.0390(5) 0.0340(5) 0.0036(4) -0.0053(4) -0.0077(4) Ag2 0.0158(6) 0.0304(6) 0.0509(7) 0.000 0.000 0.0009(5) B1 0.033(10) 0.024(9) 0.038(10) 0.000 0.000 -0.004(8) F1 0.099(7) 0.043(5) 0.116(7) -0.009(5) 0.032(6) -0.035(5) F2 0.037(4) 0.109(7) 0.091(6) 0.017(5) -0.001(5) -0.023(5) F3 0.075(5) 0.078(5) 0.053(5) 0.010(4) 0.027(4) -0.019(4) F4 0.041(4) 0.065(5) 0.107(7) -0.013(5) 0.046(5) 0.003(4) F5 0.033(4) 0.054(4) 0.071(5) 0.008(4) -0.016(4) -0.014(3) F6 0.050(4) 0.076(5) 0.042(4) 0.030(4) -0.003(3) -0.017(4) F7 0.035(8) 0.104(12) 0.35(3) 0.000 0.000 0.022(8) S1 0.0388(16) 0.0321(14) 0.0331(14) 0.0036(12) 0.0011(14) 0.0008(13) S2 0.0174(12) 0.0340(13) 0.0280(13) 0.0025(11) -0.0010(11) -0.0014(11) O1 0.043(5) 0.042(4) 0.039(4) 0.000(4) 0.014(4) 0.004(4) O2 0.061(6) 0.047(5) 0.043(5) 0.020(4) -0.008(4) 0.004(4) O3 0.035(4) 0.048(5) 0.043(5) 0.008(4) -0.018(4) -0.008(4) O4 0.032(4) 0.040(4) 0.051(5) 0.006(4) 0.011(4) 0.011(3) N1 0.034(5) 0.032(5) 0.028(4) 0.002(4) -0.002(4) -0.003(4) N2 0.014(4) 0.031(4) 0.025(4) 0.002(4) -0.002(3) -0.003(3) N4 0.015(4) 0.033(5) 0.029(5) -0.009(4) -0.005(4) -0.001(4) N6 0.019(5) 0.041(5) 0.032(5) 0.007(4) -0.006(4) -0.002(4) N8 0.036(5) 0.040(5) 0.032(5) 0.006(4) 0.001(4) -0.008(4) N9 0.033(5) 0.028(5) 0.041(5) -0.002(4) -0.007(4) -0.002(4) N10 0.006(6) 0.021(6) 0.057(8) 0.000 0.000 -0.004(5) N12 0.016(6) 0.033(7) 0.028(7) 0.000 0.000 0.001(5) C1 0.058(9) 0.042(8) 0.047(8) 0.020(6) 0.011(7) -0.010(6) C2 0.022(6) 0.044(7) 0.048(7) 0.000(6) 0.006(5) -0.010(5) C3 0.017(5) 0.037(6) 0.027(5) 0.006(5) 0.006(4) 0.005(5) C4 0.022(8) 0.026(8) 0.041(9) 0.000 0.000 -0.004(6) C7 0.012(7) 0.039(8) 0.041(9) 0.000 0.000 -0.004(7) C9 0.025(6) 0.056(7) 0.027(6) 0.012(5) -0.004(5) -0.009(5) C10 0.025(6) 0.081(8) 0.017(5) 0.006(5) -0.003(5) -0.006(6) C14 0.021(5) 0.047(6) 0.021(5) 0.010(5) 0.002(5) -0.011(5) C19 0.015(5) 0.060(7) 0.026(6) -0.008(5) 0.002(4) -0.010(5) C21 0.033(6) 0.032(6) 0.044(7) 0.003(5) -0.009(6) -0.005(5) C25 0.069(9) 0.046(7) 0.030(6) 0.006(6) -0.011(7) 0.003(7) C26 0.082(10) 0.053(8) 0.037(7) 0.000(6) -0.020(7) -0.031(7) C27 0.069(8) 0.033(6) 0.031(6) 0.001(5) 0.007(6) 0.001(6) C30 0.015(8) 0.036(9) 0.028(8) 0.000 0.000 0.009(6) C31 0.024(8) 0.027(8) 0.042(9) 0.000 0.000 0.016(7) C32 0.024(8) 0.016(7) 0.044(9) 0.000 0.000 0.001(6) C34 0.021(8) 0.034(9) 0.041(9) 0.000 0.000 -0.005(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 N8 2.288(9) . ? Ag1 N2 2.294(8) . ? Ag1 N6 2.337(8) . ? Ag1 N4 2.351(8) 1_655 ? Ag2 N12 2.254(11) 1_655 ? Ag2 N9 2.307(9) . ? Ag2 N9 2.307(9) 6_557 ? Ag2 N10 2.369(10) . ? B1 F7 1.26(2) . ? B1 F10A 1.27(4) 6_557 ? B1 F10A 1.27(4) . ? B1 F9A 1.34(3) . ? B1 F10 1.34(3) 6_557 ? B1 F10 1.34(3) . ? B1 F9 1.41(3) . ? F1 C1 1.318(14) . ? F2 C1 1.294(14) . ? F3 C1 1.304(14) . ? F4 C2 1.300(12) . ? F5 C2 1.304(13) . ? F6 C2 1.314(13) . ? S1 O2 1.410(8) . ? S1 O1 1.415(8) . ? S1 N1 1.582(8) . ? S1 C1 1.845(13) . ? S2 O3 1.416(8) . ? S2 O4 1.424(8) . ? S2 N1 1.558(8) . ? S2 C2 1.809(10) . ? N2 C7 1.315(10) . ? N2 C3 1.337(12) . ? N4 C14 1.325(13) . ? N4 C9 1.330(13) . ? N4 Ag1 2.351(8) 1_455 ? N6 C14 1.315(13) . ? N6 C19 1.316(13) . ? N8 C21 1.323(13) . ? N8 C25 1.328(14) . ? N9 C21 1.323(13) . ? N9 C27 1.347(14) . ? N10 C31 1.304(17) . ? N10 C30 1.336(17) . ? N12 C31 1.321(19) . ? N12 C34 1.327(18) . ? N12 Ag2 2.254(11) 1_455 ? C3 C4 1.356(12) . ? C3 H3B 0.9500 . ? C4 C3 1.356(12) 6_557 ? C4 H4C 0.9500 . ? C7 N2 1.315(10) 6_557 ? C7 H7A 0.9500 . ? C9 C10 1.359(15) . ? C9 H9A 0.9500 . ? C10 C19 1.368(14) . ? C10 H10A 0.9500 . ? C14 H14A 0.9500 . ? C19 H19A 0.9500 . ? C21 H21A 0.9500 . ? C25 C26 1.366(16) . ? C25 H25A 0.9500 . ? C26 C27 1.366(16) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C30 C32 1.337(19) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C34 1.38(2) . ? C32 H32A 0.9500 . ? C34 H34A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Ag1 N2 119.8(3) . . ? N8 Ag1 N6 95.0(3) . . ? N2 Ag1 N6 117.1(3) . . ? N8 Ag1 N4 115.8(3) . 1_655 ? N2 Ag1 N4 94.8(3) . 1_655 ? N6 Ag1 N4 116.1(3) . 1_655 ? N12 Ag2 N9 115.1(2) 1_655 . ? N12 Ag2 N9 115.1(2) 1_655 6_557 ? N9 Ag2 N9 116.2(4) . 6_557 ? N12 Ag2 N10 118.9(4) 1_655 . ? N9 Ag2 N10 94.0(3) . . ? N9 Ag2 N10 94.0(3) 6_557 . ? F7 B1 F10A 113(2) . 6_557 ? F7 B1 F10A 113(2) . . ? F10A B1 F10A 92(3) 6_557 . ? F7 B1 F9A 114.3(19) . . ? F10A B1 F9A 111(2) 6_557 . ? F10A B1 F9A 111(2) . . ? F7 B1 F10 104.7(17) . 6_557 ? F10A B1 F10 53.4(16) 6_557 6_557 ? F10A B1 F10 137(2) . 6_557 ? F9A B1 F10 68.3(16) . 6_557 ? F7 B1 F10 104.7(17) . . ? F10A B1 F10 137(2) 6_557 . ? F10A B1 F10 53.4(16) . . ? F9A B1 F10 68.3(16) . . ? F10 B1 F10 134(3) 6_557 . ? F7 B1 F9 106(2) . . ? F10A B1 F9 48.9(17) 6_557 . ? F10A B1 F9 48.9(17) . . ? F9A B1 F9 140(2) . . ? F10 B1 F9 102.2(16) 6_557 . ? F10 B1 F9 102.2(16) . . ? O2 S1 O1 118.6(5) . . ? O2 S1 N1 108.4(5) . . ? O1 S1 N1 116.5(4) . . ? O2 S1 C1 103.9(5) . . ? O1 S1 C1 104.6(5) . . ? N1 S1 C1 102.7(5) . . ? O3 S2 O4 119.7(5) . . ? O3 S2 N1 116.9(4) . . ? O4 S2 N1 107.1(5) . . ? O3 S2 C2 103.9(5) . . ? O4 S2 C2 102.6(5) . . ? N1 S2 C2 104.4(5) . . ? S2 N1 S1 124.9(5) . . ? C7 N2 C3 116.3(9) . . ? C7 N2 Ag1 124.1(7) . . ? C3 N2 Ag1 119.4(6) . . ? C14 N4 C9 116.1(9) . . ? C14 N4 Ag1 121.1(6) . 1_455 ? C9 N4 Ag1 122.6(7) . 1_455 ? C14 N6 C19 116.6(8) . . ? C14 N6 Ag1 121.2(6) . . ? C19 N6 Ag1 122.2(7) . . ? C21 N8 C25 115.3(9) . . ? C21 N8 Ag1 120.3(7) . . ? C25 N8 Ag1 122.6(7) . . ? C21 N9 C27 114.8(9) . . ? C21 N9 Ag2 123.0(7) . . ? C27 N9 Ag2 121.9(7) . . ? C31 N10 C30 116.5(12) . . ? C31 N10 Ag2 121.3(9) . . ? C30 N10 Ag2 122.2(8) . . ? C31 N12 C34 116.1(12) . . ? C31 N12 Ag2 124.4(9) . 1_455 ? C34 N12 Ag2 119.5(9) . 1_455 ? F2 C1 F3 110.1(12) . . ? F2 C1 F1 109.5(12) . . ? F3 C1 F1 108.7(10) . . ? F2 C1 S1 109.9(8) . . ? F3 C1 S1 110.8(9) . . ? F1 C1 S1 107.8(9) . . ? F4 C2 F5 107.6(9) . . ? F4 C2 F6 109.9(10) . . ? F5 C2 F6 107.9(9) . . ? F4 C2 S2 111.3(7) . . ? F5 C2 S2 111.1(8) . . ? F6 C2 S2 109.0(8) . . ? N2 C3 C4 122.4(10) . . ? N2 C3 H3B 118.8 . . ? C4 C3 H3B 118.8 . . ? C3 C4 C3 116.7(13) 6_557 . ? C3 C4 H4C 121.6 6_557 . ? C3 C4 H4C 121.6 . . ? N2 C7 N2 126.0(13) 6_557 . ? N2 C7 H7A 117.0 6_557 . ? N2 C7 H7A 117.0 . . ? N4 C9 C10 122.0(10) . . ? N4 C9 H9A 119.0 . . ? C10 C9 H9A 119.0 . . ? C9 C10 C19 116.9(9) . . ? C9 C10 H10A 121.5 . . ? C19 C10 H10A 121.5 . . ? N6 C14 N4 126.1(8) . . ? N6 C14 H14A 117.0 . . ? N4 C14 H14A 117.0 . . ? N6 C19 C10 122.2(9) . . ? N6 C19 H19A 118.9 . . ? C10 C19 H19A 118.9 . . ? N9 C21 N8 127.6(10) . . ? N9 C21 H21A 116.2 . . ? N8 C21 H21A 116.2 . . ? N8 C25 C26 123.1(11) . . ? N8 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C25 C26 C27 116.5(11) . . ? C25 C26 H26A 121.8 . . ? C27 C26 H26A 121.8 . . ? N9 C27 C26 122.6(11) . . ? N9 C27 H27A 118.7 . . ? C26 C27 H27A 118.7 . . ? N10 C30 C32 121.1(12) . . ? N10 C30 H30A 119.4 . . ? C32 C30 H30A 119.4 . . ? N10 C31 N12 126.8(13) . . ? N10 C31 H31A 116.6 . . ? N12 C31 H31A 116.6 . . ? C30 C32 C34 118.7(12) . . ? C30 C32 H32A 120.6 . . ? C34 C32 H32A 120.6 . . ? N12 C34 C32 120.7(13) . . ? N12 C34 H34A 119.6 . . ? C32 C34 H34A 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ag1 N6 C14 N4 -178.2(8) . . . . ? Ag1 N2 C7 N2 173.9(8) . . . 6_557 ? Ag1 N8 C21 N9 165.0(9) . . . . ? Ag1 N4 C14 N6 172.3(8) . 1_655 1_655 1_655 ? Ag2 N10 C31 N12 180.0 . . . . ? Ag2 N9 C21 N8 -174.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.219 _refine_diff_density_min -1.828 _refine_diff_density_rms 0.138