# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Carlucci, Lucia' _publ_contact_author_name 'Prof. Lucia Carlucci' _publ_contact_author_email lucia.carlucci@unimi.it _publ_section_title ; The Novel Metalloligand [Fe(bppd)3] (bppd = 1,3-bis(4-pyridyl)-1,3-propanedionate) for the Crystal Engineering of Heterometallic Coordination Networks with different Silver Salts. Anionic Control of the Structures. ; # Attachment '- 1_supp776.cif' data_Fe(III)L3 _database_code_depnum_ccdc_archive 'CCDC 824472' #TrackingRef '- 1_supp776.cif' _chemical_formula_sum 'C39 H27 Fe N6 O6' _chemical_formula_weight 731.52 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 35.923(6) _cell_length_b 20.557(3) _cell_length_c 16.968(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12530(4) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7509 _cell_measurement_theta_min 2 _cell_measurement_theta_max 19 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.163 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4524 _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (Sheldrick G.M.(1996), SADABS University of Gottingen,Germany.) ; _exptl_absorpt_correction_T_min 0.816509 _exptl_absorpt_correction_T_max 1 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 9 _diffrn_reflns_number 95789 _diffrn_reflns_av_R_equivalents 0.1134 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 20.82 _reflns_number_total 6573 _reflns_number_gt 5039 _reflns_threshold_expression >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. We were able to collect only one crystal( found serentipituously) that show a very weak diffraction only up to 20 degree of theta. Furthermore the structure contains disordered solvents. and because it was difficult to refine a consistent disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. The R before squeeze was: R1 = 0.1111 for 4535 Fo > 4sig(Fo) and 0.1535 for all 6573 data 704 parameters refined Any attempt to find other single crystals were unsuccesfull, nonetheless the ratio reflection > 2sigmaI vs parameters 5039/704= 7.15 is satisfactory and so the overall shape of Thermal ellipsoids. The refined structure is an acceptable 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^)+(0.1756P)^2^+33.8207P] 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 6573 _refine_ls_number_parameters 704 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1312 _refine_ls_R_factor_gt 0.0989 _refine_ls_wR_factor_all 0.2938 _refine_ls_wR_factor_ref 0.2650 _refine_ls_goodness_of_fit_all 1.030 _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 C1 C 0.6920(3) 0.0473(8) 0.2718(7) 0.088(4) Uani 1 1 d . . . C2 C 0.6937(3) -0.0013(6) 0.2128(8) 0.090(3) Uani 1 1 d . . . H2 H 0.6762 -0.0346 0.2142 0.108 Uiso 1 1 calc R . . C3 C 0.7199(3) -0.0020(5) 0.1534(6) 0.072(3) Uani 1 1 d . . . C4 C 0.7234(3) -0.0598(5) 0.0995(7) 0.066(3) Uani 1 1 d . . . C5 C 0.7113(4) -0.1206(6) 0.1184(8) 0.104(4) Uani 1 1 d . . . H5 H 0.6989 -0.1275 0.1657 0.125 Uiso 1 1 calc R . . C6 C 0.7416(3) -0.0530(5) 0.0290(7) 0.090(3) Uani 1 1 d . . . H6 H 0.7514 -0.0130 0.0141 0.108 Uiso 1 1 calc R . . C7 C 0.7172(4) -0.1705(6) 0.0694(10) 0.117(5) Uani 1 1 d . . . H7 H 0.7093 -0.2117 0.0848 0.140 Uiso 1 1 calc R . . C8 C 0.7449(4) -0.1063(7) -0.0192(8) 0.109(4) Uani 1 1 d . . . H8 H 0.7559 -0.1001 -0.0683 0.131 Uiso 1 1 calc R . . C9 C 0.6645(4) 0.0419(8) 0.3383(10) 0.120(5) Uani 1 1 d . . . C10 C 0.6490(6) -0.0166(10) 0.3596(14) 0.232(13) Uani 1 1 d . . . H10 H 0.6542 -0.0543 0.3313 0.279 Uiso 1 1 calc R . . C11 C 0.6600(5) 0.0960(10) 0.3847(11) 0.156(6) Uani 1 1 d . . . H11 H 0.6726 0.1349 0.3756 0.187 Uiso 1 1 calc R . . C12 C 0.6255(10) -0.0179(13) 0.424(3) 0.33(3) Uani 1 1 d . . . H12 H 0.6131 -0.0565 0.4361 0.395 Uiso 1 1 calc R . . C13 C 0.6343(6) 0.0875(14) 0.4482(13) 0.202(10) Uani 1 1 d . . . H13 H 0.6275 0.1243 0.4767 0.242 Uiso 1 1 calc R . . C14 C 0.8245(3) 0.1523(4) 0.1311(5) 0.062(3) Uani 1 1 d . . . C15 C 0.8436(3) 0.1306(5) 0.1978(6) 0.069(3) Uani 1 1 d . . . H15 H 0.8692 0.1376 0.2002 0.083 Uiso 1 1 calc R . . C16 C 0.8268(3) 0.0995(4) 0.2603(6) 0.058(2) Uani 1 1 d . . . C17 C 0.8488(2) 0.0679(4) 0.3238(5) 0.050(2) Uani 1 1 d . . . C18 C 0.8328(2) 0.0221(4) 0.3711(6) 0.064(3) Uani 1 1 d . . . H18 H 0.8073 0.0141 0.3678 0.077 Uiso 1 1 calc R . . C19 C 0.8860(3) 0.0772(5) 0.3338(5) 0.066(3) Uani 1 1 d . . . H19 H 0.8985 0.1069 0.3021 0.079 Uiso 1 1 calc R . . C20 C 0.8545(3) -0.0124(5) 0.4241(6) 0.082(3) Uani 1 1 d . . . H20 H 0.8434 -0.0449 0.4540 0.098 Uiso 1 1 calc R . . C21 C 0.9055(3) 0.0430(6) 0.3905(6) 0.075(3) Uani 1 1 d . . . H21 H 0.9306 0.0518 0.3980 0.090 Uiso 1 1 calc R . . C22 C 0.8465(3) 0.1750(4) 0.0626(6) 0.064(3) Uani 1 1 d . . . C23 C 0.8273(3) 0.1891(5) -0.0068(7) 0.090(3) Uani 1 1 d . . . H23 H 0.8015 0.1853 -0.0080 0.108 Uiso 1 1 calc R . . C24 C 0.8832(4) 0.1831(6) 0.0596(7) 0.108(4) Uani 1 1 d . . . H24 H 0.8975 0.1748 0.1043 0.129 Uiso 1 1 calc R . . C25 C 0.8468(4) 0.2095(6) -0.0767(7) 0.105(4) Uani 1 1 d . . . H25 H 0.8335 0.2176 -0.1228 0.126 Uiso 1 1 calc R . . C26 C 0.9008(4) 0.2039(8) -0.0104(11) 0.146(6) Uani 1 1 d . . . H26 H 0.9265 0.2090 -0.0105 0.175 Uiso 1 1 calc R . . C27 C 0.7369(3) 0.2616(5) 0.2521(5) 0.065(2) Uani 1 1 d . . . C28 C 0.7083(3) 0.2715(4) 0.1979(5) 0.064(3) Uani 1 1 d . . . H28 H 0.6950 0.3102 0.2003 0.077 Uiso 1 1 calc R . . C29 C 0.6987(3) 0.2257(5) 0.1396(6) 0.067(3) Uani 1 1 d . . . C30 C 0.6689(3) 0.2412(6) 0.0816(6) 0.076(3) Uani 1 1 d . . . C31 C 0.6462(4) 0.1944(7) 0.0531(9) 0.120(5) Uani 1 1 d . . . H31 H 0.6489 0.1511 0.0680 0.144 Uiso 1 1 calc R . . C32 C 0.6646(4) 0.3033(7) 0.0552(7) 0.109(4) Uani 1 1 d . . . H32 H 0.6798 0.3367 0.0737 0.131 Uiso 1 1 calc R . . C33 C 0.6191(5) 0.2134(10) 0.0017(10) 0.168(8) Uani 1 1 d . . . H33 H 0.6025 0.1817 -0.0152 0.201 Uiso 1 1 calc R . . C34 C 0.6377(5) 0.3153(9) 0.0015(9) 0.140(6) Uani 1 1 d . . . H34 H 0.6355 0.3576 -0.0174 0.168 Uiso 1 1 calc R . . C35 C 0.7463(3) 0.3138(5) 0.3076(6) 0.064(3) Uani 1 1 d . . . C36 C 0.7649(3) 0.2996(6) 0.3779(8) 0.093(3) Uani 1 1 d . . . H36 H 0.7720 0.2572 0.3902 0.112 Uiso 1 1 calc R . . C37 C 0.7383(3) 0.3789(6) 0.2955(7) 0.087(3) Uani 1 1 d . . . H37 H 0.7251 0.3922 0.2512 0.104 Uiso 1 1 calc R . . C38 C 0.7726(4) 0.3511(10) 0.4290(8) 0.127(5) Uani 1 1 d . . . H38 H 0.7836 0.3409 0.4771 0.153 Uiso 1 1 calc R . . C39 C 0.7500(3) 0.4233(6) 0.3502(10) 0.101(4) Uani 1 1 d . . . H39 H 0.7460 0.4669 0.3382 0.122 Uiso 1 1 calc R . . C40 C 0.9420(2) 0.0267(4) 0.1668(5) 0.048(2) Uani 1 1 d . . . C41 C 0.9532(2) 0.0509(4) 0.0935(4) 0.048(2) Uani 1 1 d . . . H41 H 0.9377 0.0429 0.0506 0.057 Uiso 1 1 calc R . . C42 C 0.9851(2) 0.0854(4) 0.0804(5) 0.041(2) Uani 1 1 d . . . C43 C 0.9963(2) 0.1041(4) -0.0011(5) 0.055(2) Uani 1 1 d . . . C44 C 1.0277(3) 0.1399(6) -0.0093(5) 0.101(4) Uani 1 1 d . . . H44 H 1.0413 0.1530 0.0346 0.122 Uiso 1 1 calc R . . C45 C 0.9797(3) 0.0855(6) -0.0690(6) 0.089(4) Uani 1 1 d . . . H45 H 0.9588 0.0588 -0.0665 0.106 Uiso 1 1 calc R . . C46 C 1.0395(3) 0.1569(7) -0.0854(7) 0.117(5) Uani 1 1 d . . . H46 H 1.0610 0.1816 -0.0907 0.140 Uiso 1 1 calc R . . C47 C 0.9923(3) 0.1045(7) -0.1401(6) 0.100(4) Uani 1 1 d . . . H47 H 0.9792 0.0914 -0.1845 0.120 Uiso 1 1 calc R . . C48 C 0.9085(2) -0.0137(4) 0.1741(4) 0.043(2) Uani 1 1 d . . . C49 C 0.8773(3) -0.0044(6) 0.1269(6) 0.081(3) Uani 1 1 d . . . H49 H 0.8782 0.0259 0.0863 0.097 Uiso 1 1 calc R . . C50 C 0.9050(3) -0.0596(5) 0.2298(5) 0.071(3) Uani 1 1 d . . . H50 H 0.9246 -0.0676 0.2641 0.086 Uiso 1 1 calc R . . C51 C 0.8457(3) -0.0387(6) 0.1388(7) 0.091(4) Uani 1 1 d . . . H51 H 0.8252 -0.0298 0.1071 0.109 Uiso 1 1 calc R . . C52 C 0.8724(4) -0.0951(6) 0.2368(7) 0.094(4) Uani 1 1 d . . . H52 H 0.8714 -0.1284 0.2739 0.112 Uiso 1 1 calc R . . C53 C 0.9657(3) 0.2323(5) 0.2448(6) 0.075(3) Uani 1 1 d . . . C54 C 1.0000 0.2625(8) 0.2500 0.150(9) Uani 1 2 d S . . H54 H 1.0000 0.3078 0.2500 0.180 Uiso 1 2 calc SR . . C55 C 0.9313(3) 0.2712(5) 0.2391(8) 0.093(4) Uani 1 1 d . . . C56 C 0.9013(4) 0.2600(6) 0.2793(9) 0.107(4) Uani 1 1 d . . . H56 H 0.9009 0.2253 0.3145 0.128 Uiso 1 1 calc R . . C57 C 0.9272(5) 0.3196(8) 0.1814(11) 0.155(6) Uani 1 1 d . . . H57 H 0.9460 0.3290 0.1454 0.186 Uiso 1 1 calc R . . C58 C 0.8690(4) 0.2994(8) 0.2711(12) 0.140(6) Uani 1 1 d . . . H58 H 0.8483 0.2869 0.3005 0.169 Uiso 1 1 calc R . . C59 C 0.8924(7) 0.3539(11) 0.1813(14) 0.189(9) Uani 1 1 d . . . H59 H 0.8889 0.3843 0.1414 0.227 Uiso 1 1 calc R . . N1 N 0.6199(7) 0.0328(16) 0.4690(16) 0.263(13) Uani 1 1 d . . . N2 N 0.7341(4) -0.1638(5) -0.0020(8) 0.123(4) Uani 1 1 d . . . N3 N 0.8896(3) -0.0012(5) 0.4336(5) 0.080(3) Uani 1 1 d . . . N4 N 0.8821(4) 0.2166(7) -0.0759(7) 0.132(4) Uani 1 1 d . . . N6 N 0.6145(4) 0.2719(10) -0.0260(8) 0.152(6) Uani 1 1 d . . . N7 N 0.8424(3) -0.0837(5) 0.1928(7) 0.094(3) Uani 1 1 d . . . N8 N 1.0214(3) 0.1395(6) -0.1500(5) 0.108(3) Uani 1 1 d . . . N9 N 0.8653(4) 0.3468(9) 0.2307(13) 0.185(8) Uani 1 1 d . . . O1 O 0.7137(2) 0.0952(4) 0.2745(4) 0.083(2) Uani 1 1 d . . . O2 O 0.74378(17) 0.0419(3) 0.1435(4) 0.0665(17) Uani 1 1 d . . . O3 O 0.79188(17) 0.0911(3) 0.2678(3) 0.0593(16) Uani 1 1 d . . . O4 O 0.78945(17) 0.1497(3) 0.1223(4) 0.0680(17) Uani 1 1 d . . . O5 O 0.75568(17) 0.2089(3) 0.2584(4) 0.0751(19) Uani 1 1 d . . . O6 O 0.71234(17) 0.1690(3) 0.1335(4) 0.0738(18) Uani 1 1 d . . . O7 O 0.95989(14) 0.0363(3) 0.2294(3) 0.0528(15) Uani 1 1 d . . . O8 O 1.00808(14) 0.1011(3) 0.1349(3) 0.0540(15) Uani 1 1 d . . . O9 O 0.96132(14) 0.1723(3) 0.2444(3) 0.0558(15) Uani 1 1 d . . . Fe1 Fe 0.75076(4) 0.12534(6) 0.19930(8) 0.0634(5) Uani 1 1 d . . . Fe2 Fe 1.0000 0.10118(8) 0.2500 0.0464(5) Uani 1 2 d S . . N5 N 0.7659(4) 0.4114(7) 0.4154(9) 0.128(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.064(8) 0.108(11) 0.092(9) 0.022(8) 0.019(7) 0.048(8) C2 0.061(7) 0.076(8) 0.134(10) 0.013(8) 0.028(7) 0.003(6) C3 0.053(6) 0.075(8) 0.089(8) 0.037(7) -0.015(6) -0.010(6) C4 0.065(6) 0.048(7) 0.085(8) 0.003(6) -0.016(6) -0.011(5) C5 0.132(11) 0.073(9) 0.108(10) -0.001(8) -0.004(8) -0.050(8) C6 0.121(10) 0.058(8) 0.092(9) 0.016(7) -0.025(8) -0.014(6) C7 0.157(13) 0.065(9) 0.127(12) -0.002(9) -0.016(10) -0.051(8) C8 0.160(13) 0.069(9) 0.099(9) -0.009(8) -0.014(8) -0.027(8) C9 0.085(9) 0.114(12) 0.160(13) 0.027(11) 0.050(9) 0.034(9) C10 0.23(2) 0.162(19) 0.30(3) 0.048(17) 0.21(2) 0.007(16) C11 0.121(13) 0.177(18) 0.169(16) -0.025(14) 0.056(12) -0.003(12) C12 0.35(4) 0.15(2) 0.49(6) 0.04(3) 0.27(4) 0.06(2) C13 0.19(2) 0.24(3) 0.176(19) -0.021(19) 0.090(17) 0.028(19) C14 0.091(8) 0.035(5) 0.059(6) -0.002(4) 0.014(6) 0.002(5) C15 0.064(6) 0.077(7) 0.067(7) 0.015(6) -0.005(6) -0.016(5) C16 0.059(7) 0.038(5) 0.076(7) -0.007(5) -0.007(5) 0.006(5) C17 0.036(5) 0.056(6) 0.058(5) 0.003(5) -0.005(4) 0.007(4) C18 0.041(5) 0.066(6) 0.085(7) 0.024(6) -0.011(5) -0.001(5) C19 0.051(6) 0.081(7) 0.067(6) 0.014(5) 0.008(5) -0.001(5) C20 0.065(8) 0.099(9) 0.081(8) 0.021(6) -0.004(6) 0.000(6) C21 0.033(5) 0.132(10) 0.060(6) 0.010(7) -0.003(5) -0.009(6) C22 0.056(7) 0.064(6) 0.072(7) 0.012(5) -0.008(6) 0.004(5) C23 0.089(8) 0.081(8) 0.100(9) -0.005(7) 0.026(8) 0.000(6) C24 0.097(10) 0.132(11) 0.095(9) 0.047(8) 0.021(8) -0.008(8) C25 0.109(10) 0.133(11) 0.074(8) 0.023(7) 0.001(8) -0.006(9) C26 0.093(10) 0.185(16) 0.159(15) 0.052(13) 0.016(11) -0.005(10) C27 0.060(6) 0.070(7) 0.065(6) -0.001(6) -0.003(5) 0.007(5) C28 0.072(7) 0.048(6) 0.073(6) -0.004(5) -0.011(6) 0.024(5) C29 0.062(6) 0.066(7) 0.072(7) -0.001(6) 0.001(5) 0.010(6) C30 0.068(7) 0.082(8) 0.078(7) 0.000(6) -0.023(6) 0.036(6) C31 0.095(10) 0.113(11) 0.152(13) -0.022(10) -0.038(9) 0.001(9) C32 0.126(11) 0.117(11) 0.085(8) 0.001(7) -0.052(8) 0.047(8) C33 0.147(14) 0.173(18) 0.183(17) -0.018(13) -0.120(13) 0.052(13) C34 0.168(15) 0.147(15) 0.105(11) -0.011(10) -0.056(11) 0.073(13) C35 0.060(6) 0.060(7) 0.072(7) -0.006(6) 0.002(5) -0.004(5) C36 0.093(8) 0.078(8) 0.109(10) 0.001(8) -0.024(7) 0.004(6) C37 0.083(8) 0.087(10) 0.091(8) -0.001(7) -0.012(6) 0.010(7) C38 0.157(14) 0.143(14) 0.081(9) -0.007(10) -0.032(9) -0.035(12) C39 0.110(10) 0.061(8) 0.134(11) -0.026(9) -0.039(9) 0.029(7) C40 0.051(6) 0.049(5) 0.044(6) 0.007(4) 0.008(5) -0.003(4) C41 0.037(5) 0.065(6) 0.040(5) -0.006(4) -0.011(4) -0.016(4) C42 0.036(5) 0.044(5) 0.044(5) -0.001(4) -0.001(4) -0.010(4) C43 0.037(5) 0.078(6) 0.049(6) 0.010(5) 0.005(4) -0.023(5) C44 0.122(10) 0.150(11) 0.032(6) 0.004(6) -0.002(6) -0.065(9) C45 0.074(7) 0.146(10) 0.047(7) -0.010(6) -0.013(5) -0.048(7) C46 0.111(10) 0.184(13) 0.056(8) 0.002(8) 0.004(7) -0.072(9) C47 0.089(9) 0.177(12) 0.033(6) -0.002(6) -0.011(6) -0.041(9) C48 0.046(5) 0.044(5) 0.039(5) -0.004(4) 0.003(4) -0.008(4) C49 0.073(7) 0.116(9) 0.054(6) -0.003(6) -0.006(6) -0.026(7) C50 0.084(7) 0.076(7) 0.055(6) 0.006(5) 0.007(5) -0.023(6) C51 0.048(6) 0.137(10) 0.088(8) 0.012(8) -0.004(6) -0.052(7) C52 0.119(11) 0.091(8) 0.071(8) 0.005(6) 0.030(8) -0.041(8) C53 0.062(6) 0.057(7) 0.107(8) 0.025(6) -0.014(6) -0.007(6) C54 0.098(15) 0.047(10) 0.30(3) 0.000 0.000(17) 0.000 C55 0.074(8) 0.061(7) 0.146(11) 0.028(8) 0.007(8) 0.018(6) C56 0.083(9) 0.080(9) 0.158(12) 0.015(8) 0.004(9) 0.006(8) C57 0.127(13) 0.137(14) 0.201(18) 0.038(13) 0.011(12) 0.034(11) C58 0.063(9) 0.114(12) 0.24(2) -0.002(13) 0.017(10) 0.029(9) C59 0.161(19) 0.20(2) 0.21(2) 0.074(17) -0.031(16) 0.064(18) N1 0.23(2) 0.24(3) 0.32(3) 0.09(2) 0.17(2) 0.01(2) N2 0.179(11) 0.059(8) 0.132(10) -0.026(7) -0.009(9) -0.034(7) N3 0.062(6) 0.115(8) 0.063(5) 0.015(5) -0.003(5) 0.029(5) N4 0.121(11) 0.168(12) 0.107(9) 0.040(8) 0.018(8) -0.005(9) N6 0.140(11) 0.199(16) 0.116(10) -0.043(10) -0.072(9) 0.083(12) N7 0.082(7) 0.104(8) 0.095(7) -0.004(6) 0.007(6) -0.046(6) N8 0.099(8) 0.176(10) 0.050(6) 0.014(6) 0.002(5) -0.048(8) N9 0.120(12) 0.140(13) 0.29(2) 0.077(14) 0.035(13) 0.059(11) O1 0.072(5) 0.092(6) 0.086(5) 0.002(4) 0.006(4) 0.007(4) O2 0.059(4) 0.064(4) 0.077(4) -0.004(3) -0.001(3) -0.001(4) O3 0.053(4) 0.053(4) 0.072(4) 0.011(3) -0.007(3) 0.009(3) O4 0.051(4) 0.063(4) 0.089(5) 0.011(3) -0.007(4) -0.001(3) O5 0.076(4) 0.060(4) 0.090(5) -0.001(4) -0.019(4) 0.024(4) O6 0.065(4) 0.073(5) 0.084(5) -0.010(4) -0.020(3) 0.017(4) O7 0.045(3) 0.075(4) 0.038(3) 0.004(3) -0.006(3) -0.008(3) O8 0.038(3) 0.091(4) 0.033(3) -0.002(3) -0.005(3) -0.013(3) O9 0.043(3) 0.067(5) 0.057(4) 0.006(3) 0.002(3) -0.004(3) Fe1 0.0570(9) 0.0542(9) 0.0789(10) 0.0036(7) -0.0129(7) 0.0116(6) Fe2 0.0360(10) 0.0637(12) 0.0394(10) 0.000 -0.0046(7) 0.000 N5 0.140(11) 0.106(10) 0.138(12) -0.031(9) 0.014(9) -0.015(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.256(14) . ? C1 C2 1.416(17) . ? C1 C9 1.502(17) . ? C2 C3 1.381(14) . ? C2 H2 0.9300 . ? C3 O2 1.255(11) . ? C3 C4 1.504(14) . ? C4 C5 1.362(14) . ? C4 C6 1.370(14) . ? C5 C7 1.336(17) . ? C5 H5 0.9300 . ? C6 C8 1.374(16) . ? C6 H6 0.9300 . ? C7 N2 1.362(16) . ? C7 H7 0.9300 . ? C8 N2 1.279(15) . ? C8 H8 0.9300 . ? C9 C10 1.37(2) . ? C9 C11 1.37(2) . ? C10 C12 1.39(3) . ? C10 H10 0.9300 . ? C11 C13 1.43(2) . ? C11 H11 0.9300 . ? C12 N1 1.31(4) . ? C12 H12 0.9300 . ? C13 N1 1.29(3) . ? C13 H13 0.9300 . ? C14 O4 1.269(11) . ? C14 C15 1.398(13) . ? C14 C22 1.480(13) . ? C15 C16 1.378(12) . ? C15 H15 0.9300 . ? C16 O3 1.273(10) . ? C16 C17 1.486(12) . ? C17 C19 1.360(11) . ? C17 C18 1.365(11) . ? C18 C20 1.385(12) . ? C18 H18 0.9300 . ? C19 C21 1.382(13) . ? C19 H19 0.9300 . ? C20 N3 1.294(12) . ? C20 H20 0.9300 . ? C21 N3 1.297(12) . ? C21 H21 0.9300 . ? C22 C24 1.331(14) . ? C22 C23 1.394(14) . ? C23 C25 1.438(15) . ? C23 H23 0.9300 . ? C24 C26 1.413(18) . ? C24 H24 0.9300 . ? C25 N4 1.278(15) . ? C25 H25 0.9300 . ? C26 N4 1.324(18) . ? C26 H26 0.9300 . ? C27 O5 1.279(11) . ? C27 C28 1.394(12) . ? C27 C35 1.467(13) . ? C28 C29 1.407(13) . ? C28 H28 0.9300 . ? C29 O6 1.270(11) . ? C29 C30 1.488(13) . ? C30 C31 1.351(15) . ? C30 C32 1.362(15) . ? C31 C33 1.364(18) . ? C31 H31 0.9300 . ? C32 C34 1.352(17) . ? C32 H32 0.9300 . ? C33 N6 1.30(2) . ? C33 H33 0.9300 . ? C34 N6 1.30(2) . ? C34 H34 0.9300 . ? C35 C37 1.384(14) . ? C35 C36 1.399(14) . ? C36 C38 1.397(17) . ? C36 H36 0.9300 . ? C37 C39 1.368(16) . ? C37 H37 0.9300 . ? C38 N5 1.283(18) . ? C38 H38 0.9300 . ? C39 N5 1.269(16) . ? C39 H39 0.9300 . ? C40 O7 1.256(9) . ? C40 C41 1.398(10) . ? C40 C48 1.467(11) . ? C41 C42 1.366(10) . ? C41 H41 0.9300 . ? C42 O8 1.281(9) . ? C42 C43 1.492(11) . ? C43 C44 1.354(12) . ? C43 C45 1.355(12) . ? C44 C46 1.401(14) . ? C44 H44 0.9300 . ? C45 C47 1.346(14) . ? C45 H45 0.9300 . ? C46 N8 1.323(13) . ? C46 H46 0.9300 . ? C47 N8 1.280(13) . ? C47 H47 0.9300 . ? C48 C50 1.341(12) . ? C48 C49 1.393(12) . ? C49 C51 1.351(13) . ? C49 H49 0.9300 . ? C50 C52 1.386(14) . ? C50 H50 0.9300 . ? C51 N7 1.308(13) . ? C51 H51 0.9300 . ? C52 N7 1.330(14) . ? C52 H52 0.9300 . ? C53 O9 1.243(11) . ? C53 C54 1.385(12) . ? C53 C55 1.473(14) . ? C54 C53 1.385(12) 4_755 ? C54 H54 0.9300 . ? C55 C56 1.296(15) . ? C55 C57 1.404(18) . ? C56 C58 1.422(17) . ? C56 H56 0.9300 . ? C57 C59 1.44(2) . ? C57 H57 0.9300 . ? C58 N9 1.200(19) . ? C58 H58 0.9300 . ? C59 N9 1.29(2) . ? C59 H59 0.9300 . ? O1 Fe1 1.945(8) . ? O2 Fe1 1.976(6) . ? O3 Fe1 2.007(6) . ? O4 Fe1 1.973(6) . ? O5 Fe1 1.997(7) . ? O6 Fe1 1.989(6) . ? O7 Fe2 1.995(5) . ? O8 Fe2 1.975(5) . ? O9 Fe2 2.019(6) . ? Fe2 O8 1.975(5) 4_755 ? Fe2 O7 1.995(5) 4_755 ? Fe2 O9 2.019(6) 4_755 ? 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 C1 C2 123.5(10) . . ? O1 C1 C9 116.0(14) . . ? C2 C1 C9 120.4(15) . . ? C3 C2 C1 123.5(11) . . ? C3 C2 H2 118.2 . . ? C1 C2 H2 118.2 . . ? O2 C3 C2 123.8(11) . . ? O2 C3 C4 115.5(9) . . ? C2 C3 C4 120.6(10) . . ? C5 C4 C6 116.8(11) . . ? C5 C4 C3 123.8(11) . . ? C6 C4 C3 119.3(9) . . ? C7 C5 C4 120.6(13) . . ? C7 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C4 C6 C8 118.7(11) . . ? C4 C6 H6 120.7 . . ? C8 C6 H6 120.7 . . ? C5 C7 N2 123.1(12) . . ? C5 C7 H7 118.5 . . ? N2 C7 H7 118.5 . . ? N2 C8 C6 125.1(13) . . ? N2 C8 H8 117.4 . . ? C6 C8 H8 117.4 . . ? C10 C9 C11 120.7(16) . . ? C10 C9 C1 122.0(16) . . ? C11 C9 C1 116.6(15) . . ? C9 C10 C12 118(2) . . ? C9 C10 H10 120.8 . . ? C12 C10 H10 120.8 . . ? C9 C11 C13 114.2(18) . . ? C9 C11 H11 122.9 . . ? C13 C11 H11 122.9 . . ? N1 C12 C10 123(3) . . ? N1 C12 H12 118.7 . . ? C10 C12 H12 118.7 . . ? N1 C13 C11 125(2) . . ? N1 C13 H13 117.5 . . ? C11 C13 H13 117.5 . . ? O4 C14 C15 124.8(9) . . ? O4 C14 C22 116.7(9) . . ? C15 C14 C22 118.3(10) . . ? C16 C15 C14 123.8(9) . . ? C16 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? O3 C16 C15 124.9(8) . . ? O3 C16 C17 113.1(8) . . ? C15 C16 C17 121.9(9) . . ? C19 C17 C18 116.0(8) . . ? C19 C17 C16 123.5(9) . . ? C18 C17 C16 120.2(8) . . ? C17 C18 C20 119.7(8) . . ? C17 C18 H18 120.1 . . ? C20 C18 H18 120.1 . . ? C17 C19 C21 120.9(9) . . ? C17 C19 H19 119.6 . . ? C21 C19 H19 119.6 . . ? N3 C20 C18 122.7(10) . . ? N3 C20 H20 118.7 . . ? C18 C20 H20 118.7 . . ? N3 C21 C19 121.7(8) . . ? N3 C21 H21 119.1 . . ? C19 C21 H21 119.1 . . ? C24 C22 C23 115.6(10) . . ? C24 C22 C14 126.7(10) . . ? C23 C22 C14 117.8(9) . . ? C22 C23 C25 121.2(11) . . ? C22 C23 H23 119.4 . . ? C25 C23 H23 119.4 . . ? C22 C24 C26 120.8(13) . . ? C22 C24 H24 119.6 . . ? C26 C24 H24 119.6 . . ? N4 C25 C23 120.4(12) . . ? N4 C25 H25 119.8 . . ? C23 C25 H25 119.8 . . ? N4 C26 C24 122.6(13) . . ? N4 C26 H26 118.7 . . ? C24 C26 H26 118.7 . . ? O5 C27 C28 124.4(9) . . ? O5 C27 C35 116.5(9) . . ? C28 C27 C35 119.0(9) . . ? C27 C28 C29 123.2(8) . . ? C27 C28 H28 118.4 . . ? C29 C28 H28 118.4 . . ? O6 C29 C28 125.2(9) . . ? O6 C29 C30 114.8(9) . . ? C28 C29 C30 119.9(9) . . ? C31 C30 C32 118.8(11) . . ? C31 C30 C29 121.2(11) . . ? C32 C30 C29 120.0(11) . . ? C30 C31 C33 117.1(14) . . ? C30 C31 H31 121.4 . . ? C33 C31 H31 121.4 . . ? C34 C32 C30 118.2(14) . . ? C34 C32 H32 120.9 . . ? C30 C32 H32 120.9 . . ? N6 C33 C31 125.9(17) . . ? N6 C33 H33 117.1 . . ? C31 C33 H33 117.1 . . ? N6 C34 C32 124.9(16) . . ? N6 C34 H34 117.5 . . ? C32 C34 H34 117.5 . . ? C37 C35 C36 115.3(10) . . ? C37 C35 C27 124.4(10) . . ? C36 C35 C27 120.2(10) . . ? C38 C36 C35 117.7(11) . . ? C38 C36 H36 121.1 . . ? C35 C36 H36 121.1 . . ? C39 C37 C35 118.7(11) . . ? C39 C37 H37 120.6 . . ? C35 C37 H37 120.6 . . ? N5 C38 C36 125.7(14) . . ? N5 C38 H38 117.2 . . ? C36 C38 H38 117.2 . . ? N5 C39 C37 126.9(13) . . ? N5 C39 H39 116.5 . . ? C37 C39 H39 116.5 . . ? O7 C40 C41 123.4(7) . . ? O7 C40 C48 115.9(7) . . ? C41 C40 C48 120.7(7) . . ? C42 C41 C40 124.7(7) . . ? C42 C41 H41 117.7 . . ? C40 C41 H41 117.7 . . ? O8 C42 C41 123.7(7) . . ? O8 C42 C43 115.4(6) . . ? C41 C42 C43 120.8(7) . . ? C44 C43 C45 115.7(8) . . ? C44 C43 C42 117.5(8) . . ? C45 C43 C42 126.6(8) . . ? C43 C44 C46 118.7(9) . . ? C43 C44 H44 120.6 . . ? C46 C44 H44 120.6 . . ? C47 C45 C43 122.1(9) . . ? C47 C45 H45 119.0 . . ? C43 C45 H45 119.0 . . ? N8 C46 C44 123.2(10) . . ? N8 C46 H46 118.4 . . ? C44 C46 H46 118.4 . . ? N8 C47 C45 123.8(9) . . ? N8 C47 H47 118.1 . . ? C45 C47 H47 118.1 . . ? C50 C48 C49 115.2(8) . . ? C50 C48 C40 122.3(8) . . ? C49 C48 C40 122.4(8) . . ? C51 C49 C48 121.3(10) . . ? C51 C49 H49 119.3 . . ? C48 C49 H49 119.3 . . ? C48 C50 C52 120.8(10) . . ? C48 C50 H50 119.6 . . ? C52 C50 H50 119.6 . . ? N7 C51 C49 123.3(11) . . ? N7 C51 H51 118.3 . . ? C49 C51 H51 118.3 . . ? N7 C52 C50 122.9(10) . . ? N7 C52 H52 118.6 . . ? C50 C52 H52 118.6 . . ? O9 C53 C54 123.9(10) . . ? O9 C53 C55 115.7(9) . . ? C54 C53 C55 120.4(10) . . ? C53 C54 C53 126.6(15) . 4_755 ? C53 C54 H54 116.7 . . ? C53 C54 H54 116.7 4_755 . ? C56 C55 C57 113.9(12) . . ? C56 C55 C53 124.4(11) . . ? C57 C55 C53 121.2(12) . . ? C55 C56 C58 121.8(13) . . ? C55 C56 H56 119.1 . . ? C58 C56 H56 119.1 . . ? C55 C57 C59 116.1(16) . . ? C55 C57 H57 122.0 . . ? C59 C57 H57 122.0 . . ? N9 C58 C56 127.4(16) . . ? N9 C58 H58 116.3 . . ? C56 C58 H58 116.3 . . ? N9 C59 C57 126.8(18) . . ? N9 C59 H59 116.6 . . ? C57 C59 H59 116.6 . . ? C13 N1 C12 118(3) . . ? C8 N2 C7 115.6(11) . . ? C20 N3 C21 118.9(9) . . ? C25 N4 C26 119.4(12) . . ? C33 N6 C34 114.9(14) . . ? C51 N7 C52 116.4(9) . . ? C47 N8 C46 116.3(9) . . ? C58 N9 C59 112.4(17) . . ? C1 O1 Fe1 130.6(8) . . ? C3 O2 Fe1 130.3(7) . . ? C16 O3 Fe1 128.4(6) . . ? C14 O4 Fe1 129.2(6) . . ? C27 O5 Fe1 129.8(6) . . ? C29 O6 Fe1 129.5(6) . . ? C40 O7 Fe2 128.5(5) . . ? C42 O8 Fe2 128.2(5) . . ? C53 O9 Fe2 129.2(6) . . ? O1 Fe1 O4 176.1(3) . . ? O1 Fe1 O2 87.2(3) . . ? O4 Fe1 O2 89.6(3) . . ? O1 Fe1 O6 92.1(3) . . ? O4 Fe1 O6 90.1(3) . . ? O2 Fe1 O6 92.0(3) . . ? O1 Fe1 O5 90.3(3) . . ? O4 Fe1 O5 93.0(3) . . ? O2 Fe1 O5 177.4(3) . . ? O6 Fe1 O5 87.4(3) . . ? O1 Fe1 O3 90.7(3) . . ? O4 Fe1 O3 87.4(3) . . ? O2 Fe1 O3 93.8(2) . . ? O6 Fe1 O3 173.7(3) . . ? O5 Fe1 O3 86.9(2) . . ? O8 Fe2 O8 179.9(3) 4_755 . ? O8 Fe2 O7 93.8(2) 4_755 . ? O8 Fe2 O7 86.1(2) . . ? O8 Fe2 O7 86.1(2) 4_755 4_755 ? O8 Fe2 O7 93.8(2) . 4_755 ? O7 Fe2 O7 96.0(3) . 4_755 ? O8 Fe2 O9 93.2(2) 4_755 4_755 ? O8 Fe2 O9 86.9(2) . 4_755 ? O7 Fe2 O9 171.7(2) . 4_755 ? O7 Fe2 O9 88.8(2) 4_755 4_755 ? O8 Fe2 O9 86.9(2) 4_755 . ? O8 Fe2 O9 93.2(2) . . ? O7 Fe2 O9 88.8(2) . . ? O7 Fe2 O9 171.7(2) 4_755 . ? O9 Fe2 O9 87.2(3) 4_755 . ? C39 N5 C38 115.3(13) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.401 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.073 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.500 -0.025 1412 308 ' ' 2 0.500 0.000 0.020 1412 308 ' ' # * END # Attachment '- 2a_supp799.cif' data_[Fe(III)L3Ag](BF4)_4THF _database_code_depnum_ccdc_archive 'CCDC 824473' #TrackingRef '- 2a_supp799.cif' _chemical_formula_sum 'C55 H59 Ag B F4 Fe N6 O10' _chemical_formula_weight 1214.61 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' Fe Fe 0.3463 0.8444 '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 13.246(14) _cell_length_b 22.90(2) _cell_length_c 17.291(18) _cell_angle_alpha 90.00 _cell_angle_beta 96.236(18) _cell_angle_gamma 90.00 _cell_volume 5213(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2216 _cell_measurement_theta_min 2 _cell_measurement_theta_max 27 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.060 _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2500 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (Sheldrick G.M.(1996), SADABS University of Gottingen,Germany.) ; _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 1 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 3 _diffrn_reflns_number 24643 _diffrn_reflns_av_R_equivalents 0.2382 _diffrn_reflns_av_sigmaI/netI 0.2230 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.01 _reflns_number_total 5618 _reflns_number_gt 2298 _reflns_threshold_expression >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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 BF4 anions were refined as rigid grouop and are disordered on two position with 50% occupancy giving a total of 4 BF4 per unit cell in agreement with the electroneutrality of the whole compound. ; _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^)+(0.1798P)^2^+73.8261P] 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 5618 _refine_ls_number_parameters 288 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2417 _refine_ls_R_factor_gt 0.1194 _refine_ls_wR_factor_all 0.3881 _refine_ls_wR_factor_ref 0.3169 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_restrained_S_all 1.049 _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 Fe1 Fe 0.5000 0.93724(10) 0.2500 0.0260(6) Uani 1 2 d S . . Ag1 Ag 0.5000 0.83321(6) -0.2500 0.0369(5) Uani 1 2 d S . . C1 C 0.3381(9) 1.0022(5) 0.1607(6) 0.030(3) Uani 1 1 d . . . C2 C 0.3586(9) 0.9777(6) 0.0922(6) 0.036(3) Uani 1 1 d . . . H2 H 0.3117 0.9824 0.0487 0.043 Uiso 1 1 calc R . . C3 C 0.4471(11) 0.9457(5) 0.0845(6) 0.036(3) Uani 1 1 d . . . C4 C 0.4636(10) 0.9241(5) 0.0068(6) 0.032(3) Uani 1 1 d . . . C5 C 0.5341(10) 0.8813(6) 0.0017(7) 0.046(4) Uani 1 1 d . . . H5 H 0.5721 0.8672 0.0462 0.055 Uiso 1 1 calc R . . C6 C 0.4100(10) 0.9427(6) -0.0608(7) 0.037(3) Uani 1 1 d . . . H6 H 0.3589 0.9704 -0.0597 0.044 Uiso 1 1 calc R . . C7 C 0.5480(12) 0.8592(7) -0.0700(7) 0.051(4) Uani 1 1 d . . . H7 H 0.5931 0.8284 -0.0729 0.061 Uiso 1 1 calc R . . C8 C 0.4323(10) 0.9204(6) -0.1289(7) 0.036(3) Uani 1 1 d . . . H8 H 0.3972 0.9346 -0.1746 0.043 Uiso 1 1 calc R . . C9 C 0.2485(9) 1.0395(6) 0.1641(7) 0.035(3) Uani 1 1 d . . . C10 C 0.2060(10) 1.0459(6) 0.2303(8) 0.039(3) Uani 1 1 d . . . H10 H 0.2342 1.0276 0.2756 0.047 Uiso 1 1 calc R . . C11 C 0.2038(10) 1.0676(6) 0.1005(7) 0.040(3) Uani 1 1 d . . . H11 H 0.2295 1.0632 0.0529 0.047 Uiso 1 1 calc R . . C12 C 0.1223(9) 1.0791(7) 0.2310(8) 0.043(3) Uani 1 1 d . . . H12 H 0.0928 1.0815 0.2774 0.051 Uiso 1 1 calc R . . C13 C 0.1220(10) 1.1020(6) 0.1058(8) 0.046(3) Uani 1 1 d . . . H13 H 0.0946 1.1221 0.0617 0.056 Uiso 1 1 calc R . . C14 C 0.5000 0.7957(9) 0.2500 0.049(5) Uani 1 2 d S . . H14 H 0.5000 0.7551 0.2500 0.059 Uiso 1 2 calc SR . . C15 C 0.5931(10) 0.8220(6) 0.2558(7) 0.037(3) Uani 1 1 d . . . C16 C 0.6861(10) 0.7887(5) 0.2544(8) 0.041(3) Uani 1 1 d . . . C17 C 0.6864(11) 0.7362(7) 0.2181(11) 0.066(5) Uani 1 1 d . . . H17 H 0.6267 0.7201 0.1937 0.079 Uiso 1 1 calc R . . C18 C 0.7741(11) 0.8082(7) 0.2893(8) 0.050(4) Uani 1 1 d . . . H18 H 0.7773 0.8442 0.3142 0.060 Uiso 1 1 calc R . . C19 C 0.7770(14) 0.7076(7) 0.2187(11) 0.080(6) Uani 1 1 d . . . H19 H 0.7771 0.6724 0.1921 0.096 Uiso 1 1 calc R . . C20 C 0.8596(11) 0.7754(6) 0.2883(8) 0.045(3) Uani 1 1 d . . . H20 H 0.9196 0.7895 0.3146 0.054 Uiso 1 1 calc R . . N1 N 0.0791(9) 1.1082(5) 0.1709(7) 0.049(3) Uani 1 1 d . . . N2 N 0.5005(8) 0.8797(4) -0.1344(5) 0.034(2) Uani 1 1 d . . . N3 N 0.8622(9) 0.7256(5) 0.2529(7) 0.052(3) Uani 1 1 d . . . O1 O 0.3909(6) 0.9940(3) 0.2264(5) 0.0326(19) Uani 1 1 d . . . O2 O 0.5102(6) 0.9352(3) 0.1410(5) 0.031(2) Uani 1 1 d . . . O3 O 0.6047(6) 0.8766(4) 0.2608(5) 0.034(2) Uani 1 1 d . . . O1S O 0.7969(8) 0.9735(5) 0.0847(6) 0.063(3) Uiso 1 1 d D . . C1S C 0.8992(12) 0.9905(8) 0.0819(11) 0.078(5) Uiso 1 1 d D . . H1S1 H 0.9101 1.0289 0.1051 0.093 Uiso 1 1 calc R . . H1S2 H 0.9136 0.9928 0.0282 0.093 Uiso 1 1 calc R . . C2S C 0.9658(16) 0.9496(8) 0.1228(12) 0.097(7) Uiso 1 1 d D . . H2S1 H 1.0117 0.9690 0.1622 0.116 Uiso 1 1 calc R . . H2S2 H 1.0055 0.9291 0.0874 0.116 Uiso 1 1 calc R . . C3S C 0.9001(13) 0.9101(10) 0.1576(12) 0.099(7) Uiso 1 1 d D . . H3S1 H 0.9027 0.9179 0.2129 0.119 Uiso 1 1 calc R . . H3S2 H 0.9218 0.8702 0.1507 0.119 Uiso 1 1 calc R . . C4S C 0.7979(13) 0.9179(7) 0.1212(10) 0.071(5) Uiso 1 1 d D . . H4S1 H 0.7804 0.8875 0.0831 0.085 Uiso 1 1 calc R . . H4S2 H 0.7498 0.9168 0.1597 0.085 Uiso 1 1 calc R . . O2S O 0.4027(16) 0.6592(9) 0.9683(12) 0.144(7) Uiso 1 1 d D . . C6S C 0.314(2) 0.6459(14) 1.0032(17) 0.157(12) Uiso 1 1 d D . . H6S1 H 0.3120 0.6052 1.0183 0.189 Uiso 1 1 calc R . . H6S2 H 0.2529 0.6552 0.9690 0.189 Uiso 1 1 calc R . . C7S C 0.325(3) 0.6836(15) 1.070(2) 0.206(17) Uiso 1 1 d D . . H7S1 H 0.3327 0.6599 1.1164 0.247 Uiso 1 1 calc R . . H7S2 H 0.2641 0.7068 1.0703 0.247 Uiso 1 1 calc R . . C8S C 0.411(2) 0.7218(15) 1.0703(17) 0.159(12) Uiso 1 1 d D . . H8S1 H 0.3923 0.7617 1.0812 0.191 Uiso 1 1 calc R . . H8S2 H 0.4657 0.7095 1.1084 0.191 Uiso 1 1 calc R . . C9S C 0.438(2) 0.7161(11) 0.9930(16) 0.157(12) Uiso 1 1 d D . . H9S1 H 0.5107 0.7192 0.9924 0.188 Uiso 1 1 calc R . . H9S2 H 0.4050 0.7460 0.9594 0.188 Uiso 1 1 calc R . . B1 B 0.7606(12) 0.7594(6) 0.0253(8) 0.120(5) Uiso 0.50 1 d PG A -1 F1 F 0.8403(14) 0.7650(10) 0.0844(11) 0.120(5) Uiso 0.50 1 d PG A -1 F2 F 0.7519(18) 0.7018(7) -0.0003(13) 0.120(5) Uiso 0.50 1 d PG A -1 F3 F 0.6704(13) 0.7762(10) 0.0536(12) 0.120(5) Uiso 0.50 1 d PG A -1 F4 F 0.7780(18) 0.7947(10) -0.0373(11) 0.120(5) Uiso 0.50 1 d PG A -1 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 Fe1 0.0311(14) 0.0265(14) 0.0206(12) 0.000 0.0041(9) 0.000 Ag1 0.0442(9) 0.0402(9) 0.0284(7) 0.000 0.0132(6) 0.000 C1 0.039(7) 0.030(6) 0.020(6) -0.001(5) 0.001(5) -0.003(5) C2 0.036(7) 0.052(8) 0.018(6) -0.005(6) -0.001(5) 0.013(6) C3 0.065(9) 0.034(7) 0.009(5) -0.008(5) 0.002(5) -0.015(7) C4 0.047(8) 0.025(6) 0.022(6) 0.000(5) 0.001(5) 0.001(6) C5 0.044(8) 0.057(9) 0.037(7) -0.004(7) 0.001(6) 0.022(7) C6 0.037(7) 0.045(8) 0.030(7) -0.012(6) 0.015(5) -0.001(6) C7 0.076(11) 0.059(10) 0.020(6) 0.001(6) 0.014(6) 0.040(8) C8 0.036(8) 0.035(7) 0.033(7) -0.001(6) -0.008(5) 0.004(6) C9 0.033(7) 0.040(8) 0.032(7) -0.007(5) 0.006(5) -0.004(6) C10 0.041(8) 0.036(7) 0.042(8) -0.007(6) 0.006(6) -0.006(6) C11 0.041(8) 0.059(9) 0.018(6) -0.006(6) 0.001(5) 0.013(7) C12 0.023(7) 0.062(9) 0.042(8) 0.010(7) 0.002(6) 0.003(7) C13 0.043(8) 0.052(9) 0.044(8) 0.004(7) 0.003(6) 0.014(7) C14 0.041(12) 0.031(10) 0.070(14) 0.000 -0.012(10) 0.000 C15 0.037(8) 0.038(8) 0.037(7) -0.004(6) 0.005(6) -0.005(6) C16 0.033(8) 0.028(7) 0.060(9) -0.006(6) 0.002(6) 0.003(6) C17 0.029(8) 0.056(10) 0.111(14) -0.016(10) -0.008(8) 0.006(7) C18 0.047(9) 0.046(9) 0.056(9) -0.010(7) -0.001(7) 0.012(7) C19 0.079(14) 0.053(10) 0.106(15) -0.041(10) 0.002(11) 0.026(10) C20 0.037(8) 0.048(9) 0.049(8) -0.003(7) 0.002(6) 0.005(7) N1 0.049(7) 0.057(8) 0.042(7) 0.001(6) 0.008(5) 0.005(6) N2 0.043(6) 0.032(6) 0.027(5) 0.002(4) 0.009(4) 0.001(5) N3 0.046(8) 0.044(7) 0.062(8) -0.009(6) -0.012(6) 0.006(6) O1 0.037(5) 0.029(4) 0.032(5) -0.003(4) 0.010(4) -0.006(4) O2 0.033(5) 0.017(4) 0.042(5) -0.003(3) -0.005(4) -0.001(3) O3 0.034(5) 0.034(5) 0.035(5) 0.001(4) 0.005(4) -0.001(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 Fe1 O2 1.904(9) . ? Fe1 O2 1.904(9) 2_655 ? Fe1 O1 1.954(9) 2_655 ? Fe1 O1 1.954(9) . ? Fe1 O3 1.957(9) . ? Fe1 O3 1.957(9) 2_655 ? Ag1 N2 2.264(10) . ? Ag1 N2 2.264(10) 2_654 ? Ag1 N3 2.274(12) 7_665 ? Ag1 N3 2.274(12) 8_465 ? C1 O1 1.282(13) . ? C1 C2 1.364(16) . ? C1 C9 1.468(17) . ? C2 C3 1.400(18) . ? C2 H2 0.9300 . ? C3 O2 1.239(14) . ? C3 C4 1.469(16) . ? C4 C5 1.364(18) . ? C4 C6 1.368(16) . ? C5 C7 1.369(17) . ? C5 H5 0.9300 . ? C6 C8 1.347(17) . ? C6 H6 0.9300 . ? C7 N2 1.304(15) . ? C7 H7 0.9300 . ? C8 N2 1.309(15) . ? C8 H8 0.9300 . ? C9 C10 1.337(18) . ? C9 C11 1.355(17) . ? C10 C12 1.345(18) . ? C10 H10 0.9300 . ? C11 C13 1.350(18) . ? C11 H11 0.9300 . ? C12 N1 1.313(16) . ? C12 H12 0.9300 . ? C13 N1 1.323(17) . ? C13 H13 0.9300 . ? C14 C15 1.365(15) . ? C14 C15 1.365(15) 2_655 ? C14 H14 0.9300 . ? C15 O3 1.262(14) . ? C15 C16 1.451(18) . ? C16 C18 1.330(19) . ? C16 C17 1.36(2) . ? C17 C19 1.37(2) . ? C17 H17 0.9300 . ? C18 C20 1.360(19) . ? C18 H18 0.9300 . ? C19 N3 1.28(2) . ? C19 H19 0.9300 . ? C20 N3 1.295(17) . ? C20 H20 0.9300 . ? N3 Ag1 2.274(12) 7_665 ? O1S C1S 1.416(15) . ? O1S C4S 1.421(15) . ? C1S C2S 1.422(16) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S C3S 1.432(16) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S C4S 1.441(15) . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? C4S H4S1 0.9700 . ? C4S H4S2 0.9700 . ? O2S C6S 1.414(18) . ? O2S C9S 1.432(18) . ? C6S C7S 1.430(18) . ? C6S H6S1 0.9700 . ? C6S H6S2 0.9700 . ? C7S C8S 1.430(18) . ? C7S H7S1 0.9700 . ? C7S H7S2 0.9700 . ? C8S C9S 1.427(17) . ? C8S H8S1 0.9700 . ? C8S H8S2 0.9700 . ? C9S H9S1 0.9700 . ? C9S H9S2 0.9700 . ? B1 F4 1.3902 . ? B1 F3 1.3929 . ? B1 F2 1.3932 . ? B1 F1 1.3936 . ? 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 O2 Fe1 O2 177.2(4) . 2_655 ? O2 Fe1 O1 95.3(3) . 2_655 ? O2 Fe1 O1 86.6(3) 2_655 2_655 ? O2 Fe1 O1 86.6(3) . . ? O2 Fe1 O1 95.3(3) 2_655 . ? O1 Fe1 O1 96.6(5) 2_655 . ? O2 Fe1 O3 87.2(3) . . ? O2 Fe1 O3 90.8(3) 2_655 . ? O1 Fe1 O3 87.2(4) 2_655 . ? O1 Fe1 O3 173.0(3) . . ? O2 Fe1 O3 90.8(3) . 2_655 ? O2 Fe1 O3 87.2(3) 2_655 2_655 ? O1 Fe1 O3 173.0(3) 2_655 2_655 ? O1 Fe1 O3 87.2(4) . 2_655 ? O3 Fe1 O3 89.6(5) . 2_655 ? N2 Ag1 N2 123.9(5) . 2_654 ? N2 Ag1 N3 111.9(4) . 7_665 ? N2 Ag1 N3 100.6(4) 2_654 7_665 ? N2 Ag1 N3 100.6(4) . 8_465 ? N2 Ag1 N3 111.9(4) 2_654 8_465 ? N3 Ag1 N3 107.3(6) 7_665 8_465 ? O1 C1 C2 124.7(11) . . ? O1 C1 C9 114.5(10) . . ? C2 C1 C9 120.8(10) . . ? C1 C2 C3 123.1(11) . . ? C1 C2 H2 118.4 . . ? C3 C2 H2 118.4 . . ? O2 C3 C2 121.7(11) . . ? O2 C3 C4 120.1(13) . . ? C2 C3 C4 118.2(11) . . ? C5 C4 C6 117.6(11) . . ? C5 C4 C3 118.2(11) . . ? C6 C4 C3 124.2(12) . . ? C4 C5 C7 119.0(12) . . ? C4 C5 H5 120.5 . . ? C7 C5 H5 120.5 . . ? C8 C6 C4 119.2(12) . . ? C8 C6 H6 120.4 . . ? C4 C6 H6 120.4 . . ? N2 C7 C5 122.7(13) . . ? N2 C7 H7 118.6 . . ? C5 C7 H7 118.6 . . ? N2 C8 C6 123.5(12) . . ? N2 C8 H8 118.3 . . ? C6 C8 H8 118.3 . . ? C10 C9 C11 117.0(13) . . ? C10 C9 C1 121.1(12) . . ? C11 C9 C1 121.9(11) . . ? C9 C10 C12 119.7(13) . . ? C9 C10 H10 120.2 . . ? C12 C10 H10 120.2 . . ? C13 C11 C9 120.4(12) . . ? C13 C11 H11 119.8 . . ? C9 C11 H11 119.8 . . ? N1 C12 C10 124.6(13) . . ? N1 C12 H12 117.7 . . ? C10 C12 H12 117.7 . . ? N1 C13 C11 122.9(13) . . ? N1 C13 H13 118.6 . . ? C11 C13 H13 118.6 . . ? C15 C14 C15 127.8(19) . 2_655 ? C15 C14 H14 116.1 . . ? C15 C14 H14 116.1 2_655 . ? O3 C15 C14 122.9(13) . . ? O3 C15 C16 115.1(11) . . ? C14 C15 C16 121.9(13) . . ? C18 C16 C17 117.4(13) . . ? C18 C16 C15 121.4(12) . . ? C17 C16 C15 121.2(12) . . ? C16 C17 C19 117.8(15) . . ? C16 C17 H17 121.1 . . ? C19 C17 H17 121.1 . . ? C16 C18 C20 120.0(14) . . ? C16 C18 H18 120.0 . . ? C20 C18 H18 120.0 . . ? N3 C19 C17 125.3(15) . . ? N3 C19 H19 117.4 . . ? C17 C19 H19 117.4 . . ? N3 C20 C18 123.8(13) . . ? N3 C20 H20 118.1 . . ? C18 C20 H20 118.1 . . ? C12 N1 C13 115.4(13) . . ? C7 N2 C8 117.8(11) . . ? C7 N2 Ag1 122.7(9) . . ? C8 N2 Ag1 117.5(8) . . ? C19 N3 C20 115.7(13) . . ? C19 N3 Ag1 117.8(10) . 7_665 ? C20 N3 Ag1 126.4(9) . 7_665 ? C1 O1 Fe1 127.0(8) . . ? C3 O2 Fe1 131.5(9) . . ? C15 O3 Fe1 128.1(8) . . ? C1S O1S C4S 107.4(12) . . ? O1S C1S C2S 110.2(15) . . ? O1S C1S H1S1 109.6 . . ? C2S C1S H1S1 109.6 . . ? O1S C1S H1S2 109.6 . . ? C2S C1S H1S2 109.6 . . ? H1S1 C1S H1S2 108.1 . . ? C1S C2S C3S 104.6(17) . . ? C1S C2S H2S1 110.8 . . ? C3S C2S H2S1 110.8 . . ? C1S C2S H2S2 110.8 . . ? C3S C2S H2S2 110.8 . . ? H2S1 C2S H2S2 108.9 . . ? C2S C3S C4S 108.9(17) . . ? C2S C3S H3S1 109.9 . . ? C4S C3S H3S1 109.9 . . ? C2S C3S H3S2 109.9 . . ? C4S C3S H3S2 109.9 . . ? H3S1 C3S H3S2 108.3 . . ? O1S C4S C3S 105.5(14) . . ? O1S C4S H4S1 110.6 . . ? C3S C4S H4S1 110.6 . . ? O1S C4S H4S2 110.6 . . ? C3S C4S H4S2 110.6 . . ? H4S1 C4S H4S2 108.8 . . ? C6S O2S C9S 109(2) . . ? O2S C6S C7S 101(3) . . ? O2S C6S H6S1 111.6 . . ? C7S C6S H6S1 111.6 . . ? O2S C6S H6S2 111.6 . . ? C7S C6S H6S2 111.6 . . ? H6S1 C6S H6S2 109.4 . . ? C6S C7S C8S 113(3) . . ? C6S C7S H7S1 109.0 . . ? C8S C7S H7S1 109.0 . . ? C6S C7S H7S2 109.0 . . ? C8S C7S H7S2 109.0 . . ? H7S1 C7S H7S2 107.8 . . ? C9S C8S C7S 102(3) . . ? C9S C8S H8S1 111.3 . . ? C7S C8S H8S1 111.3 . . ? C9S C8S H8S2 111.3 . . ? C7S C8S H8S2 111.3 . . ? H8S1 C8S H8S2 109.2 . . ? C8S C9S O2S 105(2) . . ? C8S C9S H9S1 110.8 . . ? O2S C9S H9S1 110.8 . . ? C8S C9S H9S2 110.8 . . ? O2S C9S H9S2 110.8 . . ? H9S1 C9S H9S2 108.8 . . ? F4 B1 F3 109.6 . . ? F4 B1 F2 108.6 . . ? F3 B1 F2 109.2 . . ? F4 B1 F1 109.9 . . ? F3 B1 F1 109.1 . . ? F2 B1 F1 110.5 . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.216 _refine_diff_density_min -1.538 _refine_diff_density_rms 0.208 # * END # Attachment '- 2c_supp797.cif' data_2c_[Fe(III)L3Ag](PF6)_4THF _database_code_depnum_ccdc_archive 'CCDC 824475' #TrackingRef '- 2c_supp797.cif' _chemical_formula_sum 'C55 H59 Ag F6 Fe N6 O10 P' _chemical_formula_weight 1272.77 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' 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' Fe Fe 0.3463 0.8444 '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 13.359(3) _cell_length_b 23.669(5) _cell_length_c 17.737(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.697(2) _cell_angle_gamma 90.00 _cell_volume 5558(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14708 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description Needle _exptl_crystal_colour red _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.060 _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2612 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;(Sheldrick G.M.(1996), SADABS University of Gottingen,Germany.) ; _exptl_absorpt_correction_T_min 0.864676 _exptl_absorpt_correction_T_max 1 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 7 _diffrn_reflns_number 42180 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.38 _reflns_number_total 6609 _reflns_number_gt 5587 _reflns_threshold_expression >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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^. ; _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^)+(0.0000P)^2^+95.2935P] 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 6609 _refine_ls_number_parameters 364 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_all 0.1669 _refine_ls_wR_factor_ref 0.1625 _refine_ls_goodness_of_fit_all 1.138 _refine_ls_restrained_S_all 1.137 _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 0.5000 0.15818(2) 0.7500 0.02382(15) Uani 1 2 d S . . Fe1 Fe 1.0000 0.42977(4) 0.7500 0.0180(2) Uani 1 2 d S . . P1 P 0.2500 0.2500 0.5000 0.0409(5) Uani 1 2 d S . . O3 O 0.8944(3) 0.36966(15) 0.7399(2) 0.0239(7) Uani 1 1 d . . . O2 O 0.8896(3) 0.48621(15) 0.72682(19) 0.0220(7) Uani 1 1 d . . . C20 C 1.0000 0.2886(3) 0.7500 0.0311(17) Uani 1 2 d S . . H20 H 1.0000 0.2493 0.7500 0.037 Uiso 1 2 calc SR . . O1 O 0.4907(3) 0.07067(15) 0.36130(18) 0.0218(7) Uani 1 1 d . . . C2 C 0.6434(4) 0.0244(2) 0.4074(3) 0.0259(11) Uani 1 1 d . . . H2 H 0.6890 0.0168 0.4506 0.031 Uiso 1 1 calc R . . N2 N 0.5032(3) 0.11461(19) 0.6355(2) 0.0258(9) Uani 1 1 d . . . C1 C 0.5573(4) 0.0561(2) 0.4150(3) 0.0218(10) Uani 1 1 d . . . C19 C 0.9071(4) 0.3161(2) 0.7454(3) 0.0256(11) Uani 1 1 d . . . F3 F 0.3328(3) 0.22397(18) 0.4534(3) 0.0557(11) Uani 1 1 d . . . C3 C 0.8362(4) 0.4965(2) 0.6628(3) 0.0192(9) Uani 1 1 d . . . C4 C 0.7464(4) 0.5331(2) 0.6659(3) 0.0229(10) Uani 1 1 d . . . N1 N 0.5772(3) 0.6021(2) 0.6744(3) 0.0329(11) Uani 1 1 d . . . O5 O 0.3000(4) 0.4702(2) 0.5850(3) 0.0499(12) Uani 1 1 d D . . C11 C 0.5671(4) 0.0724(2) 0.6288(3) 0.0271(11) Uani 1 1 d . . . H11 H 0.5990 0.0557 0.6731 0.032 Uiso 1 1 calc R . . N3 N 0.6369(3) 0.2188(2) 0.7467(3) 0.0306(10) Uani 1 1 d . . . F1 F 0.2701(3) 0.31112(17) 0.4670(3) 0.0582(11) Uani 1 1 d . . . C6 C 0.6172(4) 0.5960(3) 0.6096(3) 0.0340(13) Uani 1 1 d . . . H6 H 0.5866 0.6150 0.5667 0.041 Uiso 1 1 calc R . . C8 C 0.7061(4) 0.5398(2) 0.7333(3) 0.0269(11) Uani 1 1 d . . . H8 H 0.7343 0.5211 0.7771 0.032 Uiso 1 1 calc R . . F2 F 0.3360(3) 0.26153(19) 0.5709(3) 0.0569(11) Uani 1 1 d . . . C17 C 0.7212(4) 0.3021(2) 0.7114(3) 0.0325(12) Uani 1 1 d . . . H17 H 0.7167 0.3371 0.6872 0.039 Uiso 1 1 calc R . . C9 C 0.5400(4) 0.0760(2) 0.4932(3) 0.0224(10) Uani 1 1 d . . . C10 C 0.5890(4) 0.0519(2) 0.5596(3) 0.0261(11) Uani 1 1 d . . . H10 H 0.6352 0.0227 0.5576 0.031 Uiso 1 1 calc R . . C16 C 0.8126(4) 0.2820(2) 0.7453(3) 0.0261(11) Uani 1 1 d . . . C5 C 0.7016(4) 0.5629(2) 0.6023(3) 0.0296(12) Uani 1 1 d . . . H5 H 0.7275 0.5608 0.5562 0.036 Uiso 1 1 calc R . . C12 C 0.4728(5) 0.1191(3) 0.4995(3) 0.0353(14) Uani 1 1 d . . . H12 H 0.4376 0.1361 0.4566 0.042 Uiso 1 1 calc R . . C7 C 0.6235(4) 0.5745(3) 0.7346(3) 0.0343(13) Uani 1 1 d . . . H7 H 0.5984 0.5790 0.7807 0.041 Uiso 1 1 calc R . . C18 C 0.6355(4) 0.2694(3) 0.7137(4) 0.0353(13) Uani 1 1 d . . . H18 H 0.5738 0.2835 0.6909 0.042 Uiso 1 1 calc R . . C14 C 0.7264(5) 0.2004(3) 0.7812(4) 0.0396(14) Uani 1 1 d . . . H14 H 0.7287 0.1656 0.8058 0.048 Uiso 1 1 calc R . . C13 C 0.4591(5) 0.1366(3) 0.5733(3) 0.0386(14) Uani 1 1 d . . . H13 H 0.4147 0.1664 0.5775 0.046 Uiso 1 1 calc R . . C15 C 0.8154(4) 0.2304(3) 0.7819(4) 0.0377(14) Uani 1 1 d . . . H15 H 0.8760 0.2161 0.8065 0.045 Uiso 1 1 calc R . . C36 C 0.2940(6) 0.4159(3) 0.6183(5) 0.060(2) Uani 1 1 d D . . H36A H 0.2717 0.3881 0.5795 0.072 Uiso 1 1 calc R . . H36B H 0.2465 0.4163 0.6551 0.072 Uiso 1 1 calc R . . C37 C 0.4638(7) 0.4429(5) 0.6295(8) 0.106(4) Uani 1 1 d D . . H37A H 0.5090 0.4244 0.5987 0.127 Uiso 1 1 calc R . . H37B H 0.5040 0.4608 0.6725 0.127 Uiso 1 1 calc R . . C38 C 0.3955(8) 0.4020(5) 0.6556(8) 0.115(5) Uani 1 1 d D . . H38A H 0.3981 0.4042 0.7105 0.139 Uiso 1 1 calc R . . H38B H 0.4141 0.3641 0.6422 0.139 Uiso 1 1 calc R . . O4 O 0.6015(7) 0.3443(4) 0.5305(5) 0.106(3) Uani 1 1 d D . . C39 C 0.4022(6) 0.4846(4) 0.5845(5) 0.064(2) Uani 1 1 d D . . H41A H 0.4154 0.5220 0.6060 0.077 Uiso 1 1 calc R . . H41B H 0.4181 0.4848 0.5327 0.077 Uiso 1 1 calc R . . C43 C 0.5758(10) 0.2903(5) 0.5027(8) 0.104(4) Uani 1 1 d D . . H43A H 0.5036 0.2842 0.5002 0.125 Uiso 1 1 calc R . . H43B H 0.6106 0.2618 0.5357 0.125 Uiso 1 1 calc R . . C40 C 0.6857(11) 0.3603(6) 0.4966(9) 0.125(5) Uani 1 1 d D . . H40A H 0.7471 0.3527 0.5309 0.150 Uiso 1 1 calc R . . H40B H 0.6829 0.4004 0.4855 0.150 Uiso 1 1 calc R . . C42 C 0.6059(12) 0.2872(8) 0.4279(7) 0.145(7) Uani 1 1 d D . . H42A H 0.5495 0.2960 0.3894 0.175 Uiso 1 1 calc R . . H42B H 0.6303 0.2496 0.4183 0.175 Uiso 1 1 calc R . . C41 C 0.6858(15) 0.3285(8) 0.4270(9) 0.158(7) Uani 1 1 d D . . H41C H 0.7504 0.3100 0.4259 0.190 Uiso 1 1 calc R . . H41D H 0.6723 0.3530 0.3829 0.190 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 0.0241(3) 0.0306(3) 0.0177(3) 0.000 0.00613(19) 0.000 Fe1 0.0208(5) 0.0174(5) 0.0154(4) 0.000 0.0006(4) 0.000 P1 0.0405(13) 0.0291(11) 0.0538(14) 0.0117(10) 0.0090(11) 0.0081(10) O3 0.0231(17) 0.0224(18) 0.0249(18) -0.0024(14) -0.0011(14) -0.0035(14) O2 0.0246(18) 0.0230(18) 0.0182(16) -0.0003(13) 0.0024(13) 0.0045(14) C20 0.029(4) 0.009(3) 0.056(5) 0.000 0.008(4) 0.000 O1 0.0226(17) 0.0272(18) 0.0147(16) -0.0015(13) -0.0002(13) 0.0049(14) C2 0.025(2) 0.034(3) 0.018(2) -0.004(2) -0.0002(19) 0.004(2) N2 0.029(2) 0.028(2) 0.020(2) -0.0049(18) 0.0065(17) 0.0039(19) C1 0.027(2) 0.020(2) 0.018(2) 0.0003(18) 0.0028(18) 0.0013(19) C19 0.028(3) 0.024(3) 0.025(3) -0.001(2) 0.002(2) -0.003(2) F3 0.051(2) 0.057(3) 0.059(3) 0.009(2) 0.011(2) 0.022(2) C3 0.018(2) 0.020(2) 0.020(2) 0.0005(18) 0.0025(17) -0.0037(18) C4 0.022(2) 0.024(3) 0.023(2) 0.0001(19) 0.0023(19) -0.0027(19) N1 0.025(2) 0.037(3) 0.038(3) 0.002(2) 0.0069(19) 0.005(2) O5 0.047(3) 0.055(3) 0.047(3) 0.002(2) 0.004(2) 0.008(2) C11 0.032(3) 0.031(3) 0.018(2) 0.002(2) 0.002(2) 0.006(2) N3 0.025(2) 0.034(3) 0.033(2) 0.004(2) 0.0048(19) -0.0040(19) F1 0.065(3) 0.037(2) 0.070(3) 0.018(2) 0.002(2) 0.003(2) C6 0.031(3) 0.038(3) 0.032(3) 0.004(2) 0.004(2) 0.008(2) C8 0.031(3) 0.030(3) 0.021(2) -0.005(2) 0.006(2) -0.001(2) F2 0.050(2) 0.052(3) 0.067(3) 0.007(2) 0.000(2) 0.003(2) C17 0.032(3) 0.025(3) 0.040(3) 0.007(2) 0.006(2) 0.000(2) C9 0.022(2) 0.028(3) 0.017(2) -0.0015(19) 0.0022(18) 0.001(2) C10 0.030(3) 0.026(3) 0.022(2) 0.002(2) 0.003(2) 0.005(2) C16 0.026(3) 0.024(3) 0.029(3) 0.000(2) 0.008(2) -0.003(2) C5 0.032(3) 0.033(3) 0.025(3) 0.001(2) 0.006(2) 0.007(2) C12 0.042(3) 0.042(3) 0.020(3) -0.001(2) -0.002(2) 0.018(3) C7 0.027(3) 0.047(4) 0.030(3) -0.004(3) 0.008(2) 0.001(3) C18 0.023(3) 0.033(3) 0.048(4) 0.006(3) -0.001(2) -0.004(2) C14 0.035(3) 0.032(3) 0.051(4) 0.015(3) 0.002(3) -0.006(3) C13 0.044(3) 0.037(3) 0.037(3) -0.010(3) 0.011(3) 0.019(3) C15 0.026(3) 0.036(3) 0.049(4) 0.015(3) -0.004(3) -0.002(2) C36 0.069(5) 0.058(5) 0.053(5) -0.005(4) 0.011(4) -0.011(4) C37 0.049(6) 0.137(12) 0.126(10) 0.025(9) -0.004(6) 0.012(7) C38 0.112(10) 0.081(8) 0.137(11) 0.040(8) -0.044(9) 0.009(7) O4 0.109(6) 0.108(6) 0.104(6) -0.039(5) 0.020(5) -0.003(5) C39 0.065(5) 0.077(6) 0.052(5) -0.023(4) 0.012(4) -0.023(5) C43 0.093(9) 0.080(8) 0.138(12) -0.013(8) 0.016(8) 0.001(7) C40 0.122(12) 0.105(11) 0.153(14) 0.010(10) 0.031(11) -0.037(9) C42 0.128(13) 0.204(19) 0.094(10) -0.082(12) -0.020(9) 0.028(12) C41 0.19(2) 0.18(2) 0.113(13) 0.028(13) 0.054(13) 0.027(16) _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 2.284(4) . ? Ag1 N2 2.284(4) 2_656 ? Ag1 N3 2.332(5) . ? Ag1 N3 2.332(5) 2_656 ? Fe1 O2 1.991(3) 2_756 ? Fe1 O2 1.991(3) . ? Fe1 O1 1.995(3) 7_656 ? Fe1 O1 1.995(3) 8_556 ? Fe1 O3 1.995(4) 2_756 ? Fe1 O3 1.995(4) . ? P1 F3 1.590(4) . ? P1 F3 1.590(4) 7_556 ? P1 F1 1.597(4) . ? P1 F1 1.597(4) 7_556 ? P1 F2 1.609(4) . ? P1 F2 1.609(4) 7_556 ? O3 C19 1.280(6) . ? O2 C3 1.280(6) . ? C20 C19 1.395(6) . ? C20 C19 1.395(6) 2_756 ? C20 H20 0.9300 . ? O1 C1 1.261(6) . ? O1 Fe1 1.995(3) 7_656 ? C2 C1 1.396(7) . ? C2 C3 1.401(7) 7_656 ? C2 H2 0.9300 . ? N2 C13 1.288(8) . ? N2 C11 1.330(7) . ? C1 C9 1.512(7) . ? C19 C16 1.499(7) . ? C3 C2 1.401(7) 7_656 ? C3 C4 1.485(7) . ? C4 C8 1.384(7) . ? C4 C5 1.397(7) . ? N1 C7 1.331(8) . ? N1 C6 1.338(7) . ? O5 C39 1.408(8) . ? O5 C36 1.423(8) . ? C11 C10 1.387(7) . ? C11 H11 0.9300 . ? N3 C18 1.331(7) . ? N3 C14 1.341(8) . ? C6 C5 1.393(8) . ? C6 H6 0.9300 . ? C8 C7 1.379(8) . ? C8 H8 0.9300 . ? C17 C16 1.373(8) . ? C17 C18 1.387(8) . ? C17 H17 0.9300 . ? C9 C12 1.373(7) . ? C9 C10 1.391(7) . ? C10 H10 0.9300 . ? C16 C15 1.381(8) . ? C5 H5 0.9300 . ? C12 C13 1.409(8) . ? C12 H12 0.9300 . ? C7 H7 0.9300 . ? C18 H18 0.9300 . ? C14 C15 1.384(8) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C36 C38 1.464(10) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.447(11) . ? C37 C39 1.454(10) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? O4 C43 1.396(10) . ? O4 C40 1.397(11) . ? C39 H41A 0.9700 . ? C39 H41B 0.9700 . ? C43 C42 1.439(12) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C40 C41 1.446(13) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C42 C41 1.449(13) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C41 H41C 0.9700 . ? C41 H41D 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N2 126.3(2) . 2_656 ? N2 Ag1 N3 98.50(17) . . ? N2 Ag1 N3 114.10(16) 2_656 . ? N2 Ag1 N3 114.10(16) . 2_656 ? N2 Ag1 N3 98.50(17) 2_656 2_656 ? N3 Ag1 N3 104.0(2) . 2_656 ? O2 Fe1 O2 95.7(2) 2_756 . ? O2 Fe1 O1 93.75(14) 2_756 7_656 ? O2 Fe1 O1 86.66(14) . 7_656 ? O2 Fe1 O1 86.66(14) 2_756 8_556 ? O2 Fe1 O1 93.75(14) . 8_556 ? O1 Fe1 O1 179.4(2) 7_656 8_556 ? O2 Fe1 O3 87.97(14) 2_756 2_756 ? O2 Fe1 O3 172.88(14) . 2_756 ? O1 Fe1 O3 87.03(14) 7_656 2_756 ? O1 Fe1 O3 92.54(15) 8_556 2_756 ? O2 Fe1 O3 172.87(14) 2_756 . ? O2 Fe1 O3 87.97(15) . . ? O1 Fe1 O3 92.54(15) 7_656 . ? O1 Fe1 O3 87.03(14) 8_556 . ? O3 Fe1 O3 89.0(2) 2_756 . ? F3 P1 F3 180.0(2) . 7_556 ? F3 P1 F1 89.9(2) . . ? F3 P1 F1 90.1(2) 7_556 . ? F3 P1 F1 90.1(2) . 7_556 ? F3 P1 F1 89.9(2) 7_556 7_556 ? F1 P1 F1 179.998(1) . 7_556 ? F3 P1 F2 89.9(2) . . ? F3 P1 F2 90.1(2) 7_556 . ? F1 P1 F2 89.7(2) . . ? F1 P1 F2 90.3(2) 7_556 . ? F3 P1 F2 90.1(2) . 7_556 ? F3 P1 F2 89.9(2) 7_556 7_556 ? F1 P1 F2 90.3(2) . 7_556 ? F1 P1 F2 89.7(2) 7_556 7_556 ? F2 P1 F2 179.999(2) . 7_556 ? C19 O3 Fe1 127.9(3) . . ? C3 O2 Fe1 128.4(3) . . ? C19 C20 C19 124.3(7) . 2_756 ? C19 C20 H20 117.8 . . ? C19 C20 H20 117.8 2_756 . ? C1 O1 Fe1 127.9(3) . 7_656 ? C1 C2 C3 122.5(5) . 7_656 ? C1 C2 H2 118.8 . . ? C3 C2 H2 118.8 7_656 . ? C13 N2 C11 117.0(5) . . ? C13 N2 Ag1 121.2(4) . . ? C11 N2 Ag1 120.5(3) . . ? O1 C1 C2 125.6(5) . . ? O1 C1 C9 115.4(4) . . ? C2 C1 C9 119.0(4) . . ? O3 C19 C20 125.1(5) . . ? O3 C19 C16 115.5(5) . . ? C20 C19 C16 119.4(5) . . ? O2 C3 C2 124.7(5) . 7_656 ? O2 C3 C4 115.8(4) . . ? C2 C3 C4 119.5(4) 7_656 . ? C8 C4 C5 117.7(5) . . ? C8 C4 C3 120.6(5) . . ? C5 C4 C3 121.7(5) . . ? C7 N1 C6 116.1(5) . . ? C39 O5 C36 109.2(6) . . ? N2 C11 C10 123.7(5) . . ? N2 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? C18 N3 C14 116.9(5) . . ? C18 N3 Ag1 126.9(4) . . ? C14 N3 Ag1 116.2(4) . . ? N1 C6 C5 124.2(5) . . ? N1 C6 H6 117.9 . . ? C5 C6 H6 117.9 . . ? C7 C8 C4 119.3(5) . . ? C7 C8 H8 120.4 . . ? C4 C8 H8 120.4 . . ? C16 C17 C18 118.8(5) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C12 C9 C10 118.4(5) . . ? C12 C9 C1 119.2(4) . . ? C10 C9 C1 122.5(5) . . ? C11 C10 C9 118.3(5) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C17 C16 C15 118.7(5) . . ? C17 C16 C19 120.8(5) . . ? C15 C16 C19 120.4(5) . . ? C6 C5 C4 118.2(5) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C9 C12 C13 117.5(5) . . ? C9 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? N1 C7 C8 124.4(5) . . ? N1 C7 H7 117.8 . . ? C8 C7 H7 117.8 . . ? N3 C18 C17 123.5(5) . . ? N3 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? N3 C14 C15 123.3(6) . . ? N3 C14 H14 118.3 . . ? C15 C14 H14 118.3 . . ? N2 C13 C12 125.1(5) . . ? N2 C13 H13 117.5 . . ? C12 C13 H13 117.5 . . ? C16 C15 C14 118.7(5) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? O5 C36 C38 106.9(7) . . ? O5 C36 H36A 110.4 . . ? C38 C36 H36A 110.4 . . ? O5 C36 H36B 110.4 . . ? C38 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? C38 C37 C39 107.2(8) . . ? C38 C37 H37A 110.3 . . ? C39 C37 H37A 110.3 . . ? C38 C37 H37B 110.3 . . ? C39 C37 H37B 110.3 . . ? H37A C37 H37B 108.5 . . ? C37 C38 C36 106.9(8) . . ? C37 C38 H38A 110.3 . . ? C36 C38 H38A 110.3 . . ? C37 C38 H38B 110.3 . . ? C36 C38 H38B 110.3 . . ? H38A C38 H38B 108.6 . . ? C43 O4 C40 105.8(10) . . ? O5 C39 C37 108.1(7) . . ? O5 C39 H41A 110.1 . . ? C37 C39 H41A 110.1 . . ? O5 C39 H41B 110.1 . . ? C37 C39 H41B 110.1 . . ? H41A C39 H41B 108.4 . . ? O4 C43 C42 106.6(11) . . ? O4 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? O4 C43 H43B 110.4 . . ? C42 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? O4 C40 C41 108.6(11) . . ? O4 C40 H40A 110.0 . . ? C41 C40 H40A 110.0 . . ? O4 C40 H40B 110.0 . . ? C41 C40 H40B 110.0 . . ? H40A C40 H40B 108.4 . . ? C43 C42 C41 105.9(11) . . ? C43 C42 H42A 110.6 . . ? C41 C42 H42A 110.6 . . ? C43 C42 H42B 110.6 . . ? C41 C42 H42B 110.6 . . ? H42A C42 H42B 108.7 . . ? C40 C41 C42 104.9(12) . . ? C40 C41 H41C 110.8 . . ? C42 C41 H41C 110.8 . . ? C40 C41 H41D 110.8 . . ? C42 C41 H41D 110.8 . . ? H41C C41 H41D 108.9 . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.366 _refine_diff_density_min -1.208 _refine_diff_density_rms 0.129 # * END # Attachment '- 3_supp808.cif' data_3_[Fe(III)L3Ag](CF3SO3) _database_code_depnum_ccdc_archive 'CCDC 824476' #TrackingRef '- 3_supp808.cif' _chemical_formula_sum 'C40 H27 Ag F3 Fe N6 O9 S' _chemical_formula_weight 988.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Fe Fe 0.3463 0.8444 '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 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 20.806(3) _cell_length_b 17.767(3) _cell_length_c 25.939(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.751(2) _cell_angle_gamma 90.00 _cell_volume 9477(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4851 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3976 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;(Sheldrick G.M.(1996), SADABS University of Gottingen,Germany.) ; _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 1 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 31 _diffrn_reflns_number 48711 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.1210 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.41 _reflns_number_total 19102 _reflns_number_gt 10413 _reflns_threshold_expression >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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 crystal is unstable in air, was collected under mineral oil. Nonetheless there was a strong decay of 31% and weak diffraction. The structure contains disordered solvents. Because it was difficult to refine a consistent disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. The R before squeeze was: R1 = 0.1298 for 10733 Fo > 4sig(Fo) and 0.2000 for all 19102 data 505 parameters refined using 3209 restraints One triflate anion was refined as rigid body Only the heaviest atoms Ag,Fe and S1 were refined with anisotropic thermal parameters. One pyridil ligand is disorderd over two position 63%:27% Any attempt to search a solution in the centrosymmetric space group were unsuccesfull. The structure is non-centrosymmetric and a suitable Flack parameter was refined to 0.20(4) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(4) _refine_ls_number_reflns 19102 _refine_ls_number_parameters 505 _refine_ls_number_restraints 3209 _refine_ls_R_factor_all 0.1507 _refine_ls_R_factor_gt 0.0996 _refine_ls_wR_factor_all 0.3047 _refine_ls_wR_factor_gt 0.2708 _refine_ls_goodness_of_fit_all 0.936 _refine_ls_restrained_S_all 0.878 _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 0.87304(9) 0.01977(5) 0.91843(8) 0.0446(3) Uani 1 1 d . A . Ag2 Ag 1.08252(8) -0.52781(4) 1.21612(7) 0.0399(3) Uani 1 1 d . . . Fe2 Fe 0.93300(12) -0.47865(8) 0.86597(10) 0.0328(5) Uani 1 1 d . . . Fe1 Fe 1.02692(11) -0.02601(8) 1.26952(10) 0.0292(5) Uani 1 1 d . . . O8 O 0.8422(4) -0.4563(4) 0.8784(3) 0.0335(18) Uiso 1 1 d . . . O5 O 1.0164(4) 0.0875(4) 1.2706(3) 0.0314(19) Uiso 1 1 d . . . O7 O 0.9579(4) -0.4851(4) 0.9444(3) 0.033(2) Uiso 1 1 d . . . O12 O 0.5258(4) 0.0086(4) 0.8618(3) 0.0326(18) Uiso 1 1 d . . . O2 O 0.9334(4) -0.0400(4) 1.2751(3) 0.0335(18) Uiso 1 1 d . . . O3 O 1.1174(4) -0.0052(4) 1.2547(3) 0.0328(18) Uiso 1 1 d . . . N11 N 0.9013(3) 0.1377(3) 0.8946(3) 0.037(2) Uiso 1 1 d D . . O1 O 1.0331(3) -0.1325(4) 1.2706(3) 0.0233(16) Uiso 1 1 d . . . C78 C 0.9624(3) 0.1517(3) 0.8870(3) 0.032(2) Uiso 1 1 d D . . H78 H 0.9899 0.1108 0.8852 0.038 Uiso 1 1 calc R . . O10 O 0.8994(4) -0.4712(4) 0.7861(3) 0.032(2) Uiso 1 1 d . . . N2 N 0.6931(3) -0.0528(4) 1.2303(3) 0.033(2) Uiso 1 1 d D . . C3 C 0.9872(5) -0.1854(6) 1.2601(4) 0.027(2) Uiso 1 1 d . . . C4 C 1.0107(3) -0.2642(3) 1.2532(3) 0.027(2) Uiso 1 1 d D . . N5 N 1.0510(3) 0.3577(4) 1.2458(3) 0.041(3) Uiso 1 1 d D . . C1 C 0.8977(5) -0.0981(5) 1.2612(4) 0.024(2) Uiso 1 1 d . . . O9 O 0.9456(4) -0.3696(4) 0.8699(3) 0.0348(19) Uiso 1 1 d . . . C74 C 0.9471(3) 0.2841(3) 0.8845(3) 0.022(2) Uiso 1 1 d D . . N7 N 1.0321(5) -0.4908(5) 1.1322(3) 0.049(3) Uiso 1 1 d D . . C27 C 1.0490(5) 0.1282(6) 1.3032(4) 0.027(2) Uiso 1 1 d . . . O4 O 1.0007(4) -0.0272(4) 1.1953(3) 0.033(2) Uiso 1 1 d . . . C2 C 0.9220(5) -0.1667(6) 1.2515(4) 0.034(3) Uiso 1 1 d . . . H2 H 0.8926 -0.2038 1.2381 0.041 Uiso 1 1 calc R . . C14 C 1.1295(5) 0.0322(6) 1.2179(5) 0.033(2) Uiso 1 1 d . A . C29 C 1.0881(7) 0.0376(8) 1.3690(6) 0.049(3) Uiso 1 1 d . . . C75 C 0.8839(3) 0.2717(4) 0.8923(3) 0.041(3) Uiso 1 1 d D . . H75 H 0.8557 0.3118 0.8943 0.050 Uiso 1 1 calc R . . C28 C 1.0839(6) 0.1121(8) 1.3488(5) 0.047(3) Uiso 1 1 d . . . H28 H 1.1063 0.1505 1.3682 0.056 Uiso 1 1 calc R . . N4 N 0.9201(5) 0.0200(5) 1.0061(3) 0.055(3) Uiso 1 1 d D . . C77 C 0.8634(3) 0.1981(4) 0.8970(3) 0.038(3) Uiso 1 1 d D . . H77 H 0.8206 0.1902 0.9022 0.046 Uiso 1 1 calc R . . C76 C 0.9874(3) 0.2227(4) 0.8818(3) 0.030(2) Uiso 1 1 d D . . H76 H 1.0303 0.2292 0.8765 0.036 Uiso 1 1 calc R . . C13 C 0.7161(3) -0.1211(4) 1.2457(3) 0.048(3) Uiso 1 1 d D . . H13 H 0.6862 -0.1590 1.2489 0.057 Uiso 1 1 calc R . . C17 C 0.9926(4) 0.0069(6) 1.1056(3) 0.040(3) Uiso 1 1 d D . . C9 C 0.8264(3) -0.0824(4) 1.2523(3) 0.031(2) Uiso 1 1 d D . . C16 C 1.0274(6) 0.0081(7) 1.1568(5) 0.043(3) Uiso 1 1 d . A . C24 C 1.2294(4) 0.0724(5) 1.2765(3) 0.051(3) Uiso 1 1 d D . . H24 H 1.2178 0.0403 1.3018 0.061 Uiso 1 1 calc R . . C10 C 0.8041(3) -0.0118(4) 1.2366(4) 0.045(3) Uiso 1 1 d D . . H10 H 0.8331 0.0270 1.2331 0.054 Uiso 1 1 calc R . . N3 N 1.3049(4) 0.1632(5) 1.2518(3) 0.059(3) Uiso 1 1 d D . . C46 C 0.6748(4) -0.3341(5) 0.8528(3) 0.050(3) Uiso 1 1 d D . . H46 H 0.6473 -0.3423 0.8216 0.060 Uiso 1 1 calc R . . C22 C 1.1911(3) 0.0779(5) 1.2281(3) 0.036(3) Uiso 1 1 d D . . N8 N 0.6594(4) -0.2791(5) 0.8841(3) 0.059(3) Uiso 1 1 d D . . C47 C 0.7001(4) -0.2692(5) 0.9287(3) 0.054(3) Uiso 1 1 d D . . H47 H 0.6905 -0.2314 0.9511 0.064 Uiso 1 1 calc R . . C41 C 0.8704(7) -0.4172(8) 0.9687(6) 0.058(4) Uiso 1 1 d . . . H41 H 0.8565 -0.3938 0.9971 0.070 Uiso 1 1 calc R . . C43 C 0.7703(4) -0.3679(5) 0.9108(4) 0.057(4) Uiso 1 1 d D . . C53 C 0.9145(7) -0.3171(8) 0.8408(6) 0.055(4) Uiso 1 1 d . . . C45 C 0.7557(4) -0.3115(5) 0.9437(3) 0.051(3) Uiso 1 1 d D . . H45 H 0.7825 -0.3022 0.9751 0.061 Uiso 1 1 calc R . . C42 C 0.8313(6) -0.4169(8) 0.9200(5) 0.050(3) Uiso 1 1 d . . . C26 C 1.2852(4) 0.1158(5) 1.2864(3) 0.044(3) Uiso 1 1 d D . . H26 H 1.3105 0.1117 1.3190 0.053 Uiso 1 1 calc R . . C32 C 1.1197(5) -0.0435(6) 1.4484(4) 0.053(4) Uiso 1 1 d D . . H32 H 1.0821 -0.0713 1.4379 0.064 Uiso 1 1 calc R . . C11 C 0.7815(4) -0.1385(4) 1.2570(3) 0.045(3) Uiso 1 1 d D . . H11 H 0.7950 -0.1868 1.2675 0.054 Uiso 1 1 calc R . . C15 C 1.0893(6) 0.0395(7) 1.1706(5) 0.046(3) Uiso 1 1 d . . . H15 H 1.1050 0.0682 1.1453 0.055 Uiso 1 1 calc R A . C12 C 0.7375(4) 0.0003(4) 1.2262(3) 0.046(3) Uiso 1 1 d D . . H12 H 0.7230 0.0482 1.2156 0.055 Uiso 1 1 calc R . . C55 C 0.8674(11) -0.4110(14) 0.7706(9) 0.104(7) Uiso 1 1 d . . . C23 C 1.2104(4) 0.1265(5) 1.1918(3) 0.064(4) Uiso 1 1 d D . . H23 H 1.1859 0.1316 1.1588 0.077 Uiso 1 1 calc R . . C44 C 0.7293(4) -0.3795(5) 0.8644(3) 0.041(3) Uiso 1 1 d D . . H44 H 0.7381 -0.4168 0.8413 0.049 Uiso 1 1 calc R . . C40 C 0.9334(7) -0.4548(8) 0.9746(5) 0.048(3) Uiso 1 1 d . . . C30 C 1.1360(6) 0.0167(7) 1.4189(4) 0.080(5) Uiso 1 1 d D . . C25 C 1.2670(4) 0.1673(5) 1.2054(3) 0.057(4) Uiso 1 1 d D . . H25 H 1.2795 0.1999 1.1807 0.068 Uiso 1 1 calc R . . C54 C 0.8704(13) -0.3356(16) 0.7935(10) 0.125(8) Uiso 1 1 d . . . H54 H 0.8433 -0.2983 0.7772 0.150 Uiso 1 1 calc R . . N6 N 1.2155(6) -0.0240(8) 1.5115(5) 0.162(10) Uiso 1 1 d D . . C69 C 0.6305(3) -0.0363(4) 0.8847(3) 0.024(2) Uiso 1 1 d D . . C67 C 1.0366(5) 0.3789(6) 0.8855(4) 0.027(2) Uiso 1 1 d . . . H67 H 1.0658 0.3398 0.8947 0.032 Uiso 1 1 calc R . . C68 C 0.5599(5) -0.0488(6) 0.8778(4) 0.024(2) Uiso 1 1 d . . . O6 O 1.0556(5) -0.0172(5) 1.3416(4) 0.052(3) Uiso 1 1 d . . . O11 O 0.9242(4) 0.4061(4) 0.8632(3) 0.0266(18) Uiso 1 1 d . . . C66 C 0.9691(5) 0.3648(5) 0.8793(4) 0.021(2) Uiso 1 1 d . . . C62 C 0.9007(5) -0.1791(5) 0.8237(3) 0.060(4) Uiso 1 1 d D . . H62 H 0.8888 -0.1872 0.7881 0.072 Uiso 1 1 calc R . . N9 N 0.9195(5) -0.0909(5) 0.8949(4) 0.059(3) Uiso 1 1 d D . . C64 C 0.9029(5) -0.1069(5) 0.8444(4) 0.055(4) Uiso 1 1 d D A . H64 H 0.8922 -0.0670 0.8214 0.066 Uiso 1 1 calc R . . C71 C 0.6744(4) -0.0911(4) 0.8746(3) 0.046(3) Uiso 1 1 d D . . H71 H 0.6599 -0.1380 0.8618 0.055 Uiso 1 1 calc R . . C73 C 0.7398(4) -0.0747(5) 0.8839(4) 0.060(4) Uiso 1 1 d D A . H73 H 0.7688 -0.1119 0.8771 0.072 Uiso 1 1 calc R . . C65 C 0.9344(6) -0.1495(6) 0.9265(3) 0.105(7) Uiso 1 1 d D A . H65 H 0.9459 -0.1399 0.9619 0.126 Uiso 1 1 calc R . . C63 C 0.9340(6) -0.2238(5) 0.9100(4) 0.084(5) Uiso 1 1 d D . . H63 H 0.9451 -0.2627 0.9337 0.100 Uiso 1 1 calc R A . C72 C 0.7212(5) 0.0437(5) 0.9117(5) 0.086(6) Uiso 1 1 d D A . H72 H 0.7370 0.0901 0.9245 0.104 Uiso 1 1 calc R . . C61 C 0.9166(6) -0.2385(4) 0.8574(4) 0.061(4) Uiso 1 1 d D A . C70 C 0.6546(4) 0.0326(4) 0.9037(4) 0.059(4) Uiso 1 1 d D . . H70 H 0.6265 0.0706 0.9109 0.071 Uiso 1 1 calc R . . N12 N 0.7643(3) -0.0086(5) 0.9021(3) 0.046(3) Uiso 1 1 d D . . C35 C 1.0505(4) 0.2105(3) 1.2837(3) 0.027(2) Uiso 1 1 d D . . C39 C 1.0388(4) 0.2985(4) 1.2138(3) 0.037(3) Uiso 1 1 d D . . H39 H 1.0303 0.3076 1.1782 0.044 Uiso 1 1 calc R . . C36 C 1.0633(4) 0.2705(4) 1.3175(2) 0.051(3) Uiso 1 1 d D . . H36 H 1.0720 0.2629 1.3534 0.061 Uiso 1 1 calc R . . C37 C 1.0380(4) 0.2243(4) 1.2307(3) 0.049(3) Uiso 1 1 d D . . H37 H 1.0292 0.1850 1.2070 0.058 Uiso 1 1 calc R . . C38 C 1.0629(4) 0.3423(4) 1.2966(3) 0.034(3) Uiso 1 1 d D . . H38 H 1.0715 0.3825 1.3197 0.041 Uiso 1 1 calc R . . N1 N 1.0557(3) -0.4117(3) 1.2453(3) 0.029(2) Uiso 1 1 d D . . C7 C 0.9941(3) -0.3965(3) 1.2516(3) 0.027(2) Uiso 1 1 d D . . H7 H 0.9661 -0.4369 1.2534 0.033 Uiso 1 1 calc R . . C5 C 0.9698(3) -0.3248(4) 1.2557(3) 0.028(2) Uiso 1 1 d D . . H5 H 0.9267 -0.3175 1.2601 0.034 Uiso 1 1 calc R . . C6 C 1.0747(3) -0.2782(3) 1.2467(3) 0.034(3) Uiso 1 1 d D . . H6 H 1.1038 -0.2388 1.2449 0.040 Uiso 1 1 calc R . . C8 C 1.0941(3) -0.3523(4) 1.2431(3) 0.035(3) Uiso 1 1 d D . . H8 H 1.1370 -0.3612 1.2387 0.042 Uiso 1 1 calc R . . C50 C 1.0268(6) -0.4976(7) 1.0390(4) 0.083(5) Uiso 1 1 d D . . H50 H 1.0469 -0.5115 1.0108 0.100 Uiso 1 1 calc R . . C49 C 0.9382(5) -0.4456(7) 1.0747(5) 0.105(7) Uiso 1 1 d D . . H49 H 0.8972 -0.4236 1.0711 0.125 Uiso 1 1 calc R . . C51 C 0.9731(5) -0.4595(7) 1.1238(4) 0.084(5) Uiso 1 1 d D . . H51 H 0.9542 -0.4461 1.1527 0.101 Uiso 1 1 calc R . . C52 C 1.0574(5) -0.5091(7) 1.0897(4) 0.104(7) Uiso 1 1 d D . . H52 H 1.0985 -0.5311 1.0944 0.125 Uiso 1 1 calc R . . C48 C 0.9659(5) -0.4653(6) 1.0314(3) 0.053(4) Uiso 1 1 d D . . C31 C 1.1924(7) 0.0561(7) 1.4363(5) 0.108(7) Uiso 1 1 d D . . H31 H 1.2049 0.0967 1.4174 0.130 Uiso 1 1 calc R . . C34 C 1.1608(6) -0.0613(6) 1.4939(4) 0.065(4) Uiso 1 1 d D . . H34 H 1.1496 -0.1017 1.5135 0.077 Uiso 1 1 calc R . . C33 C 1.2302(6) 0.0337(8) 1.4825(6) 0.118(8) Uiso 1 1 d D . . H33 H 1.2681 0.0605 1.4939 0.142 Uiso 1 1 calc R . . C18B C 1.0079(7) 0.0609(8) 1.0709(5) 0.046(9) Uiso 0.368(18) 1 d PD A 1 H18B H 1.0426 0.0936 1.0802 0.055 Uiso 0.368(18) 1 calc PR A 1 C19B C 0.9406(7) -0.0405(8) 1.0899(5) 0.038(8) Uiso 0.368(18) 1 d PD A 1 H19B H 0.9290 -0.0774 1.1122 0.045 Uiso 0.368(18) 1 calc PR A 1 C20B C 0.9706(7) 0.0650(8) 1.0221(4) 0.044(9) Uiso 0.368(18) 1 d PD A 1 H20B H 0.9812 0.1014 0.9991 0.053 Uiso 0.368(18) 1 calc PR A 1 C21B C 0.9063(7) -0.0316(8) 1.0402(5) 0.076(14) Uiso 0.368(18) 1 d PD A 1 H21B H 0.8713 -0.0635 1.0299 0.091 Uiso 0.368(18) 1 calc PR A 1 C18A C 1.0229(4) 0.0039(8) 1.0618(4) 0.048(6) Uiso 0.632(18) 1 d PD A 2 H18A H 1.0676 -0.0025 1.0648 0.058 Uiso 0.632(18) 1 calc PR A 2 C19A C 0.9260(5) 0.0165(9) 1.0993(4) 0.072(8) Uiso 0.632(18) 1 d PD A 2 H19A H 0.9042 0.0188 1.1280 0.087 Uiso 0.632(18) 1 calc PR A 2 C20A C 0.9848(5) 0.0107(8) 1.0133(4) 0.076(8) Uiso 0.632(18) 1 d PD A 2 H20A H 1.0054 0.0086 0.9840 0.092 Uiso 0.632(18) 1 calc PR A 2 C21A C 0.8926(4) 0.0226(8) 1.0492(4) 0.060(7) Uiso 0.632(18) 1 d PD A 2 H21A H 0.8478 0.0289 1.0453 0.072 Uiso 0.632(18) 1 calc PR A 2 C57 C 0.8352(8) -0.4790(8) 0.6864(7) 0.091(6) Uiso 1 1 d D . . H57 H 0.8254 -0.5169 0.7087 0.109 Uiso 1 1 calc R . . C59 C 0.8180(10) -0.4859(11) 0.6329(7) 0.32(3) Uiso 1 1 d D . . H59 H 0.7965 -0.5294 0.6201 0.383 Uiso 1 1 calc R . . C56 C 0.8672(7) -0.4148(9) 0.7059(5) 0.091(6) Uiso 1 1 d D . . C58 C 0.8806(8) -0.3598(8) 0.6712(7) 0.100 Uiso 1 1 d D . . H58 H 0.9020 -0.3157 0.6831 0.120 Uiso 1 1 calc R . . C60 C 0.8615(10) -0.3720(12) 0.6185(6) 0.166(12) Uiso 1 1 d D . . H60 H 0.8709 -0.3349 0.5954 0.199 Uiso 1 1 calc R . . N10 N 0.8304(11) -0.4338(14) 0.5985(5) 0.226(14) Uiso 1 1 d D . . S1 S 0.1292(4) 0.2629(4) 0.0842(4) 0.145(3) Uani 1 1 d D . . O100 O 0.1416(9) 0.3274(7) 0.1177(6) 0.161(7) Uiso 1 1 d D . . O101 O 0.1863(7) 0.2346(10) 0.0662(8) 0.188(9) Uiso 1 1 d D . . O102 O 0.0914(9) 0.2061(8) 0.1051(8) 0.198(9) Uiso 1 1 d D . . C100 C 0.0659(9) 0.2780(11) 0.0293(9) 0.29(3) Uiso 1 1 d D . . F103 F 0.0115(9) 0.3010(11) 0.0376(8) 0.211(8) Uiso 1 1 d D . . F102 F 0.0632(10) 0.2155(10) 0.0071(9) 0.225(9) Uiso 1 1 d D . . F101 F 0.0967(13) 0.3263(14) 0.0079(13) 0.348(17) Uiso 1 1 d D . . S2 S 0.6567(4) 0.2255(5) 0.9707(3) 0.200 Uiso 1 1 d GD . . O200 O 0.6119(6) 0.1686(7) 0.9490(4) 0.200 Uiso 1 1 d GD . . O201 O 0.7200(5) 0.2193(8) 0.9560(4) 0.200 Uiso 1 1 d GD . . O202 O 0.6303(6) 0.3002(6) 0.9664(4) 0.200 Uiso 1 1 d GD . . C200 C 0.6657(5) 0.2349(6) 1.0414(3) 0.200 Uiso 1 1 d GD . . F203 F 0.6137(6) 0.2427(8) 1.0594(4) 0.200 Uiso 1 1 d GD . . F202 F 0.7046(6) 0.2880(7) 1.0524(4) 0.200 Uiso 1 1 d GD . . F201 F 0.6911(7) 0.1715(6) 1.0493(4) 0.200 Uiso 1 1 d GD . . 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 0.0272(5) 0.0219(4) 0.0802(9) 0.0032(4) -0.0060(5) -0.0071(3) Ag2 0.0279(5) 0.0143(4) 0.0760(8) -0.0017(4) 0.0036(5) 0.0027(3) Fe2 0.0259(11) 0.0191(9) 0.0531(14) 0.0018(7) 0.0047(9) 0.0038(6) Fe1 0.0204(10) 0.0110(8) 0.0555(14) -0.0007(7) 0.0038(9) -0.0038(6) S1 0.121(5) 0.100(5) 0.216(8) -0.045(5) 0.029(5) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11 2.286(6) . ? Ag1 N12 2.293(7) . ? Ag1 N9 2.313(8) . ? Ag1 N4 2.335(8) . ? Ag2 N1 2.296(6) . ? Ag2 N5 2.305(6) 1_545 ? Ag2 N2 2.317(6) 3_545 ? Ag2 N7 2.363(8) . ? Fe2 O9 1.955(8) . ? Fe2 O12 1.963(8) 3_545 ? Fe2 O8 2.004(8) . ? Fe2 O7 2.024(9) . ? Fe2 O11 2.056(7) 1_545 ? Fe2 O10 2.087(9) . ? Fe1 O6 1.880(11) . ? Fe1 O1 1.897(7) . ? Fe1 O4 1.920(9) . ? Fe1 O2 1.989(8) . ? Fe1 O3 2.012(8) . ? Fe1 O5 2.029(8) . ? O8 C42 1.332(15) . ? O5 C27 1.234(12) . ? O7 C40 1.135(15) . ? O12 C68 1.275(12) . ? O12 Fe2 1.963(8) 3_455 ? O2 C1 1.290(12) . ? O3 C14 1.219(13) . ? N11 C78 1.340(6) . ? N11 C77 1.340(6) . ? O1 C3 1.338(12) . ? C78 C76 1.379(5) . ? C78 H78 0.9300 . ? O10 C55 1.29(2) . ? N2 C12 1.336(6) . ? N2 C13 1.343(6) . ? N2 Ag2 2.317(6) 3_455 ? C3 C2 1.382(15) . ? C3 C4 1.501(12) . ? C4 C5 1.380(5) . ? C4 C6 1.391(5) . ? N5 C38 1.332(6) . ? N5 C39 1.340(6) . ? N5 Ag2 2.305(6) 1_565 ? C1 C2 1.358(15) . ? C1 C9 1.493(12) . ? O9 C53 1.307(16) . ? C74 C75 1.378(5) . ? C74 C76 1.384(5) . ? C74 C66 1.517(11) . ? N7 C52 1.331(6) . ? N7 C51 1.334(6) . ? C27 C28 1.323(16) . ? C27 C35 1.550(12) . ? O4 C16 1.366(15) . ? C2 H2 0.9300 . ? C14 C15 1.383(17) . ? C14 C22 1.507(13) . ? C29 O6 1.329(16) . ? C29 C28 1.421(18) . ? C29 C30 1.553(17) . ? C75 C77 1.387(5) . ? C75 H75 0.9300 . ? C28 H28 0.9300 . ? N4 C21A 1.333(7) . ? N4 C21B 1.334(7) . ? N4 C20B 1.335(7) . ? N4 C20A 1.339(7) . ? C77 H77 0.9300 . ? C76 H76 0.9300 . ? C13 C11 1.382(6) . ? C13 H13 0.9300 . ? C17 C18A 1.380(6) . ? C17 C19A 1.382(6) . ? C17 C19B 1.383(6) . ? C17 C18B 1.384(6) . ? C17 C16 1.413(15) . ? C9 C10 1.377(5) . ? C9 C11 1.384(6) . ? C16 C15 1.398(18) . ? C24 C22 1.384(6) . ? C24 C26 1.384(6) . ? C24 H24 0.9300 . ? C10 C12 1.387(6) . ? C10 H10 0.9300 . ? N3 C25 1.336(6) . ? N3 C26 1.340(6) . ? C46 N8 1.340(6) . ? C46 C44 1.386(6) . ? C46 H46 0.9300 . ? C22 C23 1.381(6) . ? N8 C47 1.337(6) . ? C47 C45 1.384(6) . ? C47 H47 0.9300 . ? C41 C42 1.397(19) . ? C41 C40 1.456(19) . ? C41 H41 0.9300 . ? C43 C45 1.378(6) . ? C43 C44 1.381(6) . ? C43 C42 1.529(15) . ? C53 C54 1.45(3) . ? C53 C61 1.461(16) . ? C45 H45 0.9300 . ? C26 H26 0.9300 . ? C32 C34 1.386(6) . ? C32 C30 1.387(6) . ? C32 H32 0.9300 . ? C11 H11 0.9300 . ? C15 H15 0.9300 . ? C12 H12 0.9300 . ? C55 C54 1.46(3) . ? C55 C56 1.68(3) . ? C23 C25 1.382(6) . ? C23 H23 0.9300 . ? C44 H44 0.9300 . ? C40 C48 1.537(16) . ? C30 C31 1.383(6) . ? C25 H25 0.9300 . ? C54 H54 0.9300 . ? N6 C33 1.334(7) . ? N6 C34 1.335(7) . ? C69 C70 1.384(6) . ? C69 C71 1.386(5) . ? C69 C68 1.470(12) . ? C67 C68 1.397(14) 3 ? C67 C66 1.413(14) . ? C67 H67 0.9300 . ? C68 C67 1.397(14) 3_445 ? O11 C66 1.210(11) . ? O11 Fe2 2.056(7) 1_565 ? C62 C61 1.377(6) . ? C62 C64 1.389(6) . ? C62 H62 0.9300 . ? N9 C65 1.333(6) . ? N9 C64 1.334(6) . ? C64 H64 0.9300 . ? C71 C73 1.378(6) . ? C71 H71 0.9300 . ? C73 N12 1.337(6) . ? C73 H73 0.9300 . ? C65 C63 1.387(6) . ? C65 H65 0.9300 . ? C63 C61 1.384(6) . ? C63 H63 0.9300 . ? C72 N12 1.341(6) . ? C72 C70 1.385(6) . ? C72 H72 0.9300 . ? C70 H70 0.9300 . ? C35 C36 1.379(6) . ? C35 C37 1.382(6) . ? C39 C37 1.389(6) . ? C39 H39 0.9300 . ? C36 C38 1.386(6) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? N1 C8 1.328(6) . ? N1 C7 1.344(6) . ? C7 C5 1.381(5) . ? C7 H7 0.9300 . ? C5 H5 0.9300 . ? C6 C8 1.385(5) . ? C6 H6 0.9300 . ? C8 H8 0.9300 . ? C50 C48 1.379(6) . ? C50 C52 1.387(6) . ? C50 H50 0.9300 . ? C49 C48 1.384(6) . ? C49 C51 1.388(6) . ? C49 H49 0.9300 . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C31 C33 1.387(6) . ? C31 H31 0.9300 . ? C34 H34 0.9300 . ? C33 H33 0.9300 . ? C18B C20B 1.383(6) . ? C18B H18B 0.9300 . ? C19B C21B 1.386(6) . ? C19B H19B 0.9300 . ? C20B H20B 0.9300 . ? C21B H21B 0.9300 . ? C18A C20A 1.386(6) . ? C18A H18A 0.9300 . ? C19A C21A 1.381(6) . ? C19A H19A 0.9300 . ? C20A H20A 0.9300 . ? C21A H21A 0.9300 . ? C57 C56 1.377(6) . ? C57 C59 1.386(6) . ? C57 H57 0.9300 . ? C59 N10 1.337(7) . ? C59 H59 0.9300 . ? C56 C58 1.385(6) . ? C58 C60 1.383(6) . ? C58 H58 0.9300 . ? C60 N10 1.339(7) . ? C60 H60 0.9300 . ? S1 O101 1.432(6) . ? S1 O102 1.436(7) . ? S1 O100 1.437(6) . ? S1 C100 1.81(2) . ? C100 F102 1.249(8) . ? C100 F101 1.250(8) . ? C100 F103 1.252(8) . ? S2 O201 1.4310 . ? S2 O200 1.4315 . ? S2 O202 1.4350 . ? S2 C200 1.8226 . ? C200 F201 1.2479 . ? C200 F202 1.2487 . ? C200 F203 1.2488 . ? 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 N11 Ag1 N12 116.0(3) . . ? N11 Ag1 N9 124.9(3) . . ? N12 Ag1 N9 101.8(3) . . ? N11 Ag1 N4 100.1(3) . . ? N12 Ag1 N4 115.9(3) . . ? N9 Ag1 N4 97.4(3) . . ? N1 Ag2 N5 125.9(3) . 1_545 ? N1 Ag2 N2 113.9(3) . 3_545 ? N5 Ag2 N2 96.0(3) 1_545 3_545 ? N1 Ag2 N7 87.6(3) . . ? N5 Ag2 N7 116.4(3) 1_545 . ? N2 Ag2 N7 119.4(3) 3_545 . ? O9 Fe2 O12 89.5(3) . 3_545 ? O9 Fe2 O8 85.3(3) . . ? O12 Fe2 O8 172.2(3) 3_545 . ? O9 Fe2 O7 89.5(3) . . ? O12 Fe2 O7 86.9(4) 3_545 . ? O8 Fe2 O7 87.3(3) . . ? O9 Fe2 O11 177.3(3) . 1_545 ? O12 Fe2 O11 88.0(3) 3_545 1_545 ? O8 Fe2 O11 97.0(3) . 1_545 ? O7 Fe2 O11 89.2(3) . 1_545 ? O9 Fe2 O10 90.6(3) . . ? O12 Fe2 O10 97.8(3) 3_545 . ? O8 Fe2 O10 88.0(3) . . ? O7 Fe2 O10 175.3(4) . . ? O11 Fe2 O10 90.8(3) 1_545 . ? O6 Fe1 O1 93.3(3) . . ? O6 Fe1 O4 175.4(4) . . ? O1 Fe1 O4 90.7(3) . . ? O6 Fe1 O2 96.0(4) . . ? O1 Fe1 O2 86.5(3) . . ? O4 Fe1 O2 86.6(4) . . ? O6 Fe1 O3 90.6(4) . . ? O1 Fe1 O3 97.1(3) . . ? O4 Fe1 O3 86.6(4) . . ? O2 Fe1 O3 172.3(3) . . ? O6 Fe1 O5 85.5(3) . . ? O1 Fe1 O5 177.0(3) . . ? O4 Fe1 O5 90.6(3) . . ? O2 Fe1 O5 90.8(3) . . ? O3 Fe1 O5 85.7(3) . . ? C42 O8 Fe2 121.0(8) . . ? C27 O5 Fe1 122.9(7) . . ? C40 O7 Fe2 126.5(9) . . ? C68 O12 Fe2 125.2(7) . 3_455 ? C1 O2 Fe1 127.4(7) . . ? C14 O3 Fe1 124.1(8) . . ? C78 N11 C77 115.9(5) . . ? C78 N11 Ag1 119.9(4) . . ? C77 N11 Ag1 123.0(4) . . ? C3 O1 Fe1 130.8(6) . . ? N11 C78 C76 124.4(4) . . ? N11 C78 H78 117.8 . . ? C76 C78 H78 117.8 . . ? C55 O10 Fe2 116.1(12) . . ? C12 N2 C13 116.2(5) . . ? C12 N2 Ag2 122.3(5) . 3_455 ? C13 N2 Ag2 121.4(5) . 3_455 ? O1 C3 C2 121.1(9) . . ? O1 C3 C4 116.4(8) . . ? C2 C3 C4 122.2(9) . . ? C5 C4 C6 118.3(3) . . ? C5 C4 C3 120.6(6) . . ? C6 C4 C3 121.1(6) . . ? C38 N5 C39 116.1(5) . . ? C38 N5 Ag2 119.5(4) . 1_565 ? C39 N5 Ag2 121.5(5) . 1_565 ? O2 C1 C2 123.8(10) . . ? O2 C1 C9 114.2(8) . . ? C2 C1 C9 121.9(9) . . ? C53 O9 Fe2 128.8(8) . . ? C75 C74 C76 118.7(3) . . ? C75 C74 C66 118.1(6) . . ? C76 C74 C66 123.2(6) . . ? C52 N7 C51 115.9(5) . . ? C52 N7 Ag2 121.2(6) . . ? C51 N7 Ag2 122.3(6) . . ? O5 C27 C28 131.0(11) . . ? O5 C27 C35 111.5(8) . . ? C28 C27 C35 117.4(10) . . ? C16 O4 Fe1 130.0(8) . . ? C1 C2 C3 124.7(11) . . ? C1 C2 H2 117.6 . . ? C3 C2 H2 117.6 . . ? O3 C14 C15 125.1(11) . . ? O3 C14 C22 115.4(10) . . ? C15 C14 C22 119.3(10) . . ? O6 C29 C28 119.1(13) . . ? O6 C29 C30 118.8(11) . . ? C28 C29 C30 121.6(12) . . ? C74 C75 C77 118.6(4) . . ? C74 C75 H75 120.7 . . ? C77 C75 H75 120.7 . . ? C27 C28 C29 121.8(13) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C21A N4 C21B 45.9(8) . . ? C21A N4 C20B 97.7(7) . . ? C21B N4 C20B 116.3(5) . . ? C21A N4 C20A 115.9(5) . . ? C21B N4 C20A 97.8(7) . . ? C20B N4 C20A 46.0(8) . . ? C21A N4 Ag1 130.4(6) . . ? C21B N4 Ag1 122.9(6) . . ? C20B N4 Ag1 119.9(6) . . ? C20A N4 Ag1 113.6(6) . . ? N11 C77 C75 124.0(4) . . ? N11 C77 H77 118.0 . . ? C75 C77 H77 118.0 . . ? C78 C76 C74 118.4(4) . . ? C78 C76 H76 120.8 . . ? C74 C76 H76 120.8 . . ? N2 C13 C11 124.1(5) . . ? N2 C13 H13 118.0 . . ? C11 C13 H13 118.0 . . ? C18A C17 C19A 118.9(3) . . ? C18A C17 C19B 99.7(7) . . ? C19A C17 C19B 46.6(8) . . ? C18A C17 C18B 46.7(8) . . ? C19A C17 C18B 99.5(6) . . ? C19B C17 C18B 118.5(3) . . ? C18A C17 C16 122.8(9) . . ? C19A C17 C16 118.0(9) . . ? C19B C17 C16 123.5(9) . . ? C18B C17 C16 117.7(9) . . ? C10 C9 C11 118.7(4) . . ? C10 C9 C1 119.8(6) . . ? C11 C9 C1 121.4(6) . . ? O4 C16 C15 117.2(11) . . ? O4 C16 C17 118.2(11) . . ? C15 C16 C17 124.5(12) . . ? C22 C24 C26 118.6(4) . . ? C22 C24 H24 120.7 . . ? C26 C24 H24 120.7 . . ? C9 C10 C12 118.7(4) . . ? C9 C10 H10 120.7 . . ? C12 C10 H10 120.7 . . ? C25 N3 C26 116.0(5) . . ? N8 C46 C44 123.8(5) . . ? N8 C46 H46 118.1 . . ? C44 C46 H46 118.1 . . ? C23 C22 C24 118.4(4) . . ? C23 C22 C14 123.1(7) . . ? C24 C22 C14 118.5(7) . . ? C47 N8 C46 116.2(5) . . ? N8 C47 C45 124.3(5) . . ? N8 C47 H47 117.8 . . ? C45 C47 H47 117.8 . . ? C42 C41 C40 119.2(13) . . ? C42 C41 H41 120.4 . . ? C40 C41 H41 120.4 . . ? C45 C43 C44 118.8(4) . . ? C45 C43 C42 125.1(8) . . ? C44 C43 C42 116.0(8) . . ? O9 C53 C54 121.3(16) . . ? O9 C53 C61 121.5(12) . . ? C54 C53 C61 116.8(16) . . ? C43 C45 C47 118.3(4) . . ? C43 C45 H45 120.8 . . ? C47 C45 H45 120.8 . . ? O8 C42 C41 125.7(12) . . ? O8 C42 C43 114.4(10) . . ? C41 C42 C43 119.9(12) . . ? N3 C26 C24 124.0(5) . . ? N3 C26 H26 118.0 . . ? C24 C26 H26 118.0 . . ? C34 C32 C30 118.4(4) . . ? C34 C32 H32 120.8 . . ? C30 C32 H32 120.8 . . ? C13 C11 C9 118.4(4) . . ? C13 C11 H11 120.8 . . ? C9 C11 H11 120.8 . . ? C14 C15 C16 126.8(13) . . ? C14 C15 H15 116.6 . . ? C16 C15 H15 116.6 . . ? N2 C12 C10 123.9(5) . . ? N2 C12 H12 118.1 . . ? C10 C12 H12 118.1 . . ? O10 C55 C54 130(2) . . ? O10 C55 C56 101.6(16) . . ? C54 C55 C56 115.8(19) . . ? C22 C23 C25 118.5(4) . . ? C22 C23 H23 120.7 . . ? C25 C23 H23 120.7 . . ? C43 C44 C46 118.6(4) . . ? C43 C44 H44 120.7 . . ? C46 C44 H44 120.7 . . ? O7 C40 C41 129.5(14) . . ? O7 C40 C48 115.2(12) . . ? C41 C40 C48 114.4(12) . . ? C31 C30 C32 118.5(4) . . ? C31 C30 C29 123.8(10) . . ? C32 C30 C29 117.6(10) . . ? N3 C25 C23 124.4(5) . . ? N3 C25 H25 117.8 . . ? C23 C25 H25 117.8 . . ? C53 C54 C55 122(2) . . ? C53 C54 H54 118.9 . . ? C55 C54 H54 118.9 . . ? C33 N6 C34 116.5(5) . . ? C70 C69 C71 118.4(4) . . ? C70 C69 C68 118.5(7) . . ? C71 C69 C68 123.0(7) . . ? C68 C67 C66 120.4(9) 3 . ? C68 C67 H67 119.8 3 . ? C66 C67 H67 119.8 . . ? O12 C68 C67 126.5(10) . 3_445 ? O12 C68 C69 114.5(8) . . ? C67 C68 C69 118.9(9) 3_445 . ? C29 O6 Fe1 130.7(9) . . ? C66 O11 Fe2 122.2(7) . 1_565 ? O11 C66 C67 129.3(9) . . ? O11 C66 C74 112.2(8) . . ? C67 C66 C74 117.7(8) . . ? C61 C62 C64 118.2(4) . . ? C61 C62 H62 120.9 . . ? C64 C62 H62 120.9 . . ? C65 N9 C64 116.0(5) . . ? C65 N9 Ag1 124.7(6) . . ? C64 N9 Ag1 112.7(6) . . ? N9 C64 C62 124.4(5) . . ? N9 C64 H64 117.8 . . ? C62 C64 H64 117.8 . . ? C73 C71 C69 118.7(4) . . ? C73 C71 H71 120.6 . . ? C69 C71 H71 120.6 . . ? N12 C73 C71 124.1(5) . . ? N12 C73 H73 117.9 . . ? C71 C73 H73 117.9 . . ? N9 C65 C63 124.4(5) . . ? N9 C65 H65 117.8 . . ? C63 C65 H65 117.8 . . ? C61 C63 C65 118.1(4) . . ? C61 C63 H63 120.9 . . ? C65 C63 H63 120.9 . . ? N12 C72 C70 123.8(5) . . ? N12 C72 H72 118.1 . . ? C70 C72 H72 118.1 . . ? C62 C61 C63 118.9(4) . . ? C62 C61 C53 123.6(9) . . ? C63 C61 C53 117.5(9) . . ? C69 C70 C72 118.6(4) . . ? C69 C70 H70 120.7 . . ? C72 C70 H70 120.7 . . ? C73 N12 C72 116.4(5) . . ? C73 N12 Ag1 124.8(5) . . ? C72 N12 Ag1 118.8(5) . . ? C36 C35 C37 119.0(4) . . ? C36 C35 C27 122.2(6) . . ? C37 C35 C27 118.8(6) . . ? N5 C39 C37 124.1(4) . . ? N5 C39 H39 118.0 . . ? C37 C39 H39 118.0 . . ? C35 C36 C38 118.3(4) . . ? C35 C36 H36 120.9 . . ? C38 C36 H36 120.9 . . ? C35 C37 C39 118.1(4) . . ? C35 C37 H37 120.9 . . ? C39 C37 H37 120.9 . . ? N5 C38 C36 124.4(4) . . ? N5 C38 H38 117.8 . . ? C36 C38 H38 117.8 . . ? C8 N1 C7 115.9(5) . . ? C8 N1 Ag2 121.4(4) . . ? C7 N1 Ag2 120.3(4) . . ? N1 C7 C5 124.1(4) . . ? N1 C7 H7 117.9 . . ? C5 C7 H7 117.9 . . ? C4 C5 C7 118.8(4) . . ? C4 C5 H5 120.6 . . ? C7 C5 H5 120.6 . . ? C8 C6 C4 118.2(4) . . ? C8 C6 H6 120.9 . . ? C4 C6 H6 120.9 . . ? N1 C8 C6 124.7(4) . . ? N1 C8 H8 117.7 . . ? C6 C8 H8 117.7 . . ? C48 C50 C52 118.4(4) . . ? C48 C50 H50 120.8 . . ? C52 C50 H50 120.8 . . ? C48 C49 C51 118.3(4) . . ? C48 C49 H49 120.8 . . ? C51 C49 H49 120.8 . . ? N7 C51 C49 124.4(5) . . ? N7 C51 H51 117.8 . . ? C49 C51 H51 117.8 . . ? N7 C52 C50 124.5(5) . . ? N7 C52 H52 117.8 . . ? C50 C52 H52 117.8 . . ? C50 C48 C49 118.5(4) . . ? C50 C48 C40 116.7(9) . . ? C49 C48 C40 124.8(9) . . ? C30 C31 C33 118.6(4) . . ? C30 C31 H31 120.7 . . ? C33 C31 H31 120.7 . . ? N6 C34 C32 124.1(5) . . ? N6 C34 H34 117.9 . . ? C32 C34 H34 117.9 . . ? N6 C33 C31 124.0(5) . . ? N6 C33 H33 118.0 . . ? C31 C33 H33 118.0 . . ? C20B C18B C17 118.6(4) . . ? C20B C18B H18B 120.7 . . ? C17 C18B H18B 120.7 . . ? C17 C19B C21B 118.3(4) . . ? C17 C19B H19B 120.9 . . ? C21B C19B H19B 120.9 . . ? N4 C20B C18B 124.0(5) . . ? N4 C20B H20B 118.0 . . ? C18B C20B H20B 118.0 . . ? N4 C21B C19B 124.2(5) . . ? N4 C21B H21B 117.9 . . ? C19B C21B H21B 117.9 . . ? C17 C18A C20A 118.3(4) . . ? C17 C18A H18A 120.9 . . ? C20A C18A H18A 120.9 . . ? C21A C19A C17 118.2(4) . . ? C21A C19A H19A 120.9 . . ? C17 C19A H19A 120.9 . . ? N4 C20A C18A 124.2(5) . . ? N4 C20A H20A 117.9 . . ? C18A C20A H20A 117.9 . . ? N4 C21A C19A 124.7(5) . . ? N4 C21A H21A 117.7 . . ? C19A C21A H21A 117.7 . . ? C56 C57 C59 118.5(4) . . ? C56 C57 H57 120.7 . . ? C59 C57 H57 120.7 . . ? N10 C59 C57 124.1(5) . . ? N10 C59 H59 117.9 . . ? C57 C59 H59 117.9 . . ? C57 C56 C58 118.6(4) . . ? C57 C56 C55 109.2(13) . . ? C58 C56 C55 130.6(13) . . ? C60 C58 C56 118.5(4) . . ? C60 C58 H58 120.8 . . ? C56 C58 H58 120.8 . . ? N10 C60 C58 124.1(5) . . ? N10 C60 H60 117.9 . . ? C58 C60 H60 117.9 . . ? C59 N10 C60 116.1(5) . . ? O101 S1 O102 113.9(7) . . ? O101 S1 O100 113.3(7) . . ? O102 S1 O100 113.0(7) . . ? O101 S1 C100 109.7(12) . . ? O102 S1 C100 91.5(12) . . ? O100 S1 C100 113.6(11) . . ? F102 C100 F101 113.3(10) . . ? F102 C100 F103 113.0(10) . . ? F101 C100 F103 113.0(10) . . ? F102 C100 S1 102.0(16) . . ? F101 C100 S1 95(2) . . ? F103 C100 S1 118.9(17) . . ? O201 S2 O200 114.2 . . ? O201 S2 O202 114.1 . . ? O200 S2 O202 113.8 . . ? O201 S2 C200 108.6 . . ? O200 S2 C200 115.0 . . ? O202 S2 C200 88.5 . . ? F201 C200 F202 113.6 . . ? F201 C200 F203 114.1 . . ? F202 C200 F203 113.6 . . ? F201 C200 S2 93.4 . . ? F202 C200 S2 105.2 . . ? F203 C200 S2 115.1 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.592 _refine_diff_density_min -1.854 _refine_diff_density_rms 0.183 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.858 0.008 0.112 947 390 ' ' 2 0.850 -0.016 0.612 947 390 ' ' 3 0.716 0.250 0.845 24 4 ' ' 4 0.216 0.250 0.345 24 4 ' ' 5 0.216 0.750 0.845 24 4 ' ' 6 0.716 0.750 0.345 24 4 ' ' # * END # Attachment '- 4_supp806.cif' data_4_[Fe(III)2L6Ag3](NO3)3 _database_code_depnum_ccdc_archive 'CCDC 824477' #TrackingRef '- 4_supp806.cif' _chemical_formula_sum 'C78 H54 Ag3 Fe2 N15 O21' _chemical_formula_weight 1972.67 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 20.341(3) _cell_length_b 17.552(3) _cell_length_c 26.677(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.888(2) _cell_angle_gamma 90.00 _cell_volume 9503(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4393 _cell_measurement_theta_min 2 _cell_measurement_theta_max 22 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.040 _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3952 _exptl_absorpt_coefficient_mu 0.975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;(Sheldrick G.M.(1996), SADABS University of Gottingen,Germany.) ; _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 45990 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.41 _reflns_number_total 8737 _reflns_number_gt 5271 _reflns_threshold_expression >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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 crystal is unstable in air, was collected under mineral oil. The structure contains disordered solvents. Because it was difficult to refine a consistent disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. The R before squeeze was: R1 = 0.1134 for 9420 Fo > 4sig(Fo) 532 parameters refined using 219 restraints Three pyridil ligand were found disorderd over two position with occupancy 82%:18%; 83:17% and 50%:50. Both the nitrate anions and all the atoms with occupancy equal or lower than 50% were refined isotropically. One Silver atom is disordered over two position (50%-50%) following the disorder of one pyridil ligand (50%-50%) and the disordered "dimer" is bridged by a nitrate anion ; _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^)+(0.1444P)^2^+447.1804P] 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_number_reflns 8737 _refine_ls_number_parameters 532 _refine_ls_number_restraints 219 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0886 _refine_ls_wR_factor_all 0.2611 _refine_ls_wR_factor_gt 0.2328 _refine_ls_goodness_of_fit_all 0.774 _refine_ls_restrained_S_all 0.774 _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 0.64485(3) 0.49736(4) 0.61926(3) 0.0301(2) Uani 1 1 d . A . Fe1 Fe 0.79468(5) 0.49764(6) 0.94804(4) 0.0230(3) Uani 1 1 d . . . O3 O 0.8874(3) 0.4785(3) 0.9323(2) 0.0254(13) Uani 1 1 d . . . O6 O 0.6942(3) 0.1100(3) 0.5464(2) 0.0229(13) Uani 1 1 d . . . C30 C 0.7148(4) 0.2384(4) 0.5643(3) 0.0219(17) Uani 1 1 d . A . N4 N 0.7026(4) 0.4852(4) 0.6949(3) 0.0356(19) Uani 1 1 d D . . O5 O 0.2999(3) 0.5134(3) 0.5451(2) 0.0244(13) Uani 1 1 d . . . C1 C 0.6871(4) 0.8368(4) 0.5279(3) 0.0270(19) Uani 1 1 d . . . O2 O 0.7800(3) 0.3842(3) 0.9452(2) 0.0236(12) Uani 1 1 d . . . N5 N 0.5372(4) 0.5274(4) 0.5977(3) 0.0363(19) Uani 1 1 d D . . C9 C 0.6881(4) 0.7557(5) 0.5467(4) 0.028(2) Uani 1 1 d . A . C35 C 0.4047(4) 0.5579(4) 0.5715(4) 0.031(2) Uani 1 1 d D . . N3 N 1.0781(4) 0.3063(5) 0.9261(4) 0.044(2) Uani 1 1 d . . . C29 C 0.7397(4) 0.1597(4) 0.5583(4) 0.028(2) Uani 1 1 d . . . N1 N 0.6900(4) 0.6089(4) 0.5854(3) 0.0362(19) Uani 1 1 d . . . C27 C 0.3343(4) 0.5714(4) 0.5597(3) 0.0246(18) Uani 1 1 d . . . C13 C 0.7077(6) 0.6686(6) 0.6139(5) 0.053(3) Uani 1 1 d . A . H115 H 0.7199 0.6603 0.6477 0.063 Uiso 1 1 calc R . . C15 C 0.8655(5) 0.4335(5) 0.8494(4) 0.034(2) Uani 1 1 d . . . H116 H 0.8820 0.4050 0.8237 0.041 Uiso 1 1 calc R . . N6 N 0.6656(4) 0.3855(4) 0.5765(3) 0.0323(18) Uani 1 1 d . . . C14 C 0.9015(4) 0.4380(5) 0.8949(3) 0.0260(19) Uani 1 1 d . . . C26 C 1.0411(5) 0.2961(6) 0.8837(4) 0.043(3) Uani 1 1 d . . . H26 H 1.0548 0.2603 0.8609 0.052 Uiso 1 1 calc R . . C31 C 0.6505(5) 0.2516(5) 0.5728(4) 0.037(2) Uani 1 1 d . . . H27 H 0.6218 0.2107 0.5750 0.045 Uiso 1 1 calc R A . C17 C 0.7712(4) 0.4741(5) 0.7894(4) 0.033(2) Uani 1 1 d D . . C16 C 0.8050(4) 0.4704(5) 0.8406(3) 0.030(2) Uani 1 1 d . A . C12 C 0.6722(5) 0.6230(6) 0.5376(4) 0.043(3) Uani 1 1 d . A . H30 H 0.6608 0.5819 0.5168 0.052 Uiso 1 1 calc R . . O4 O 0.7754(3) 0.5053(3) 0.8738(2) 0.0287(13) Uani 1 1 d . . . C33 C 0.6278(5) 0.3235(5) 0.5782(5) 0.045(3) Uani 1 1 d . A . H34 H 0.5834 0.3301 0.5834 0.054 Uiso 1 1 calc R . . C34 C 0.7290(4) 0.3729(5) 0.5674(3) 0.0281(19) Uani 1 1 d . A . H35 H 0.7566 0.4147 0.5651 0.034 Uiso 1 1 calc R . . C32 C 0.7552(4) 0.3009(5) 0.5614(3) 0.0255(18) Uani 1 1 d . . . H36 H 0.7994 0.2949 0.5555 0.031 Uiso 1 1 calc R A . C24 C 0.9820(4) 0.3363(6) 0.8710(4) 0.036(2) Uani 1 1 d . . . H37 H 0.9565 0.3261 0.8415 0.043 Uiso 1 1 calc R . . C18A C 0.7286(7) 0.5334(7) 0.7773(4) 0.045(4) Uani 0.831(12) 1 d P A 1 H58 H 0.7205 0.5706 0.8010 0.055 Uiso 0.831(12) 1 calc PR A 1 C19A C 0.7811(6) 0.4218(7) 0.7504(4) 0.042(3) Uani 0.831(12) 1 d P A 1 H32 H 0.8115 0.3824 0.7554 0.051 Uiso 0.831(12) 1 calc PR A 1 C20A C 0.6985(6) 0.5368(7) 0.7298(4) 0.042(3) Uani 0.831(12) 1 d P A 1 H41 H 0.6729 0.5796 0.7217 0.051 Uiso 0.831(12) 1 calc PR A 1 C21A C 0.7452(7) 0.4297(7) 0.7049(4) 0.046(4) Uani 0.831(12) 1 d P A 1 H46 H 0.7514 0.3940 0.6799 0.055 Uiso 0.831(12) 1 calc PR A 1 C21B C 0.7679(8) 0.5057(19) 0.706(2) 0.055(18) Uiso 0.169(12) 1 d PD A 2 H21B H 0.7896 0.5246 0.6791 0.066 Uiso 0.169(12) 1 calc PR A 2 C19B C 0.805(2) 0.5022(19) 0.7508(12) 0.052(17) Uiso 0.169(12) 1 d PD A 2 H19B H 0.8489 0.5174 0.7545 0.062 Uiso 0.169(12) 1 calc PR A 2 C18B C 0.7065(8) 0.4518(19) 0.7835(17) 0.045(16) Uiso 0.169(12) 1 d PD A 2 H18B H 0.6852 0.4331 0.8107 0.055 Uiso 0.169(12) 1 calc PR A 2 C20B C 0.673(2) 0.4575(18) 0.7371(11) 0.042(15) Uiso 0.169(12) 1 d PD A 2 H20B H 0.6296 0.4422 0.7336 0.050 Uiso 0.169(12) 1 calc PR A 2 C36A C 0.4245(5) 0.4872(6) 0.5849(5) 0.041(3) Uani 0.819(12) 1 d P A 1 H54 H 0.3946 0.4471 0.5844 0.049 Uiso 0.819(12) 1 calc PR A 1 C37A C 0.4518(5) 0.6143(6) 0.5647(5) 0.040(3) Uani 0.819(12) 1 d P A 1 H24 H 0.4401 0.6616 0.5511 0.048 Uiso 0.819(12) 1 calc PR A 1 C38A C 0.4902(6) 0.4751(6) 0.5996(5) 0.041(3) Uani 0.819(12) 1 d P A 1 H38 H 0.5024 0.4270 0.6116 0.050 Uiso 0.819(12) 1 calc PR A 1 C39A C 0.5169(5) 0.5965(6) 0.5791(5) 0.041(3) Uani 0.819(12) 1 d P A 1 H25 H 0.5486 0.6341 0.5759 0.050 Uiso 0.819(12) 1 calc PR A 1 C36B C 0.4380(15) 0.5855(15) 0.6141(7) 0.034(13) Uiso 0.181(12) 1 d PD A 2 H36B H 0.4140 0.6160 0.6348 0.041 Uiso 0.181(12) 1 calc PR A 2 C37B C 0.4439(19) 0.5138(13) 0.5434(14) 0.047(15) Uiso 0.181(12) 1 d PD A 2 H37B H 0.4240 0.4936 0.5140 0.056 Uiso 0.181(12) 1 calc PR A 2 C38B C 0.5028(13) 0.5730(13) 0.6296(9) 0.014(9) Uiso 0.181(12) 1 d PD A 2 H38B H 0.5223 0.5934 0.6592 0.017 Uiso 0.181(12) 1 calc PR A 2 C39B C 0.5090(19) 0.4959(17) 0.5535(8) 0.051(16) Uiso 0.181(12) 1 d PD A 2 H39B H 0.5324 0.4652 0.5325 0.062 Uiso 0.181(12) 1 calc PR A 2 C23 C 1.0024(5) 0.4033(6) 0.9482(4) 0.040(2) Uani 1 1 d . . . H39 H 0.9905 0.4396 0.9714 0.048 Uiso 1 1 calc R . . C28 C 0.8060(4) 0.1428(5) 0.5664(4) 0.030(2) Uani 1 1 d . . . H28 H 0.8340 0.1823 0.5772 0.037 Uiso 1 1 calc R . . C10 C 0.6697(5) 0.6941(5) 0.5170(4) 0.035(2) Uani 1 1 d . . . H44 H 0.6558 0.7009 0.4834 0.042 Uiso 1 1 calc R A . C2 C 0.6532(5) 0.8525(5) 0.4831(4) 0.040(3) Uani 1 1 d . . . H45 H 0.6299 0.8133 0.4666 0.048 Uiso 1 1 calc R . . C25 C 1.0595(5) 0.3601(5) 0.9572(4) 0.045(3) Uani 1 1 d . . . H47 H 1.0858 0.3694 0.9864 0.054 Uiso 1 1 calc R . . C22 C 0.9640(4) 0.3912(5) 0.9042(4) 0.029(2) Uani 1 1 d . . . C11 C 0.7091(6) 0.7421(6) 0.5958(4) 0.047(3) Uani 1 1 d . . . H52 H 0.7240 0.7819 0.6167 0.056 Uiso 1 1 calc R A . O1 O 0.8204(3) 0.4837(3) 1.0197(2) 0.0269(13) Uani 1 1 d . . . C3 C 0.6519(5) 0.9257(5) 0.4604(4) 0.052(3) Uani 1 1 d D . . N10 N 0.5000 0.1586(7) 0.2500 0.051(3) Uiso 1 2 d SD . . O11 O 0.4468(5) 0.1258(7) 0.2512(5) 0.119(4) Uiso 1 1 d D . . O12 O 0.5000 0.2291(8) 0.2500 0.121(6) Uiso 1 2 d SD . . C8A C 0.6032(6) 1.0148(6) 0.3347(4) 0.038(5) Uiso 0.50 1 d PD B 1 H8A H 0.5933 1.0651 0.3260 0.046 Uiso 0.50 1 calc PR B 1 C4A C 0.6351(4) 0.9245(6) 0.3981(4) 0.056(6) Uiso 0.50 1 d PD B 1 C5A C 0.6346(8) 0.8682(6) 0.3623(6) 0.067(7) Uiso 0.50 1 d PD B 1 H5A H 0.6454 0.8185 0.3716 0.080 Uiso 0.50 1 calc PR B 1 C7A C 0.6182(9) 0.8854(7) 0.3128(6) 0.078(8) Uiso 0.50 1 d PD B 1 H7A H 0.6181 0.8467 0.2890 0.094 Uiso 0.50 1 calc PR B 1 N2A N 0.6017(6) 0.9594(7) 0.2974(5) 0.045(4) Uiso 0.50 1 d PD . 1 C6A C 0.6191(4) 0.9967(5) 0.3840(3) 0.053(3) Uiso 0.50 1 d PD B 1 H6A H 0.6188 1.0347 0.4083 0.064 Uiso 0.50 1 calc PR B 1 C5B C 0.5496(6) 0.8965(6) 0.4102(4) 0.036(4) Uiso 0.50 1 d PD B 2 H5B H 0.5407 0.8583 0.4329 0.043 Uiso 0.50 1 calc PR B 2 C4B C 0.6059(5) 0.9392(5) 0.4175(3) 0.034(4) Uiso 0.50 1 d PD B 2 C7B C 0.5065(6) 0.9100(7) 0.3695(5) 0.049(5) Uiso 0.50 1 d PD B 2 H7B H 0.4683 0.8809 0.3653 0.059 Uiso 0.50 1 calc PR B 2 C8B C 0.5759(5) 1.0082(6) 0.3430(4) 0.049(5) Uiso 0.50 1 d PD B 2 H8B H 0.5855 1.0457 0.3199 0.059 Uiso 0.50 1 calc PR B 2 N2B N 0.5184(6) 0.9661(7) 0.3344(5) 0.040(4) Uiso 0.50 1 d PD B 2 C6B C 0.6191(4) 0.9967(5) 0.3840(3) 0.053(3) Uiso 0.50 1 d PD B 2 H6B H 0.6565 1.0268 0.3893 0.064 Uiso 0.50 1 calc PR B 2 Ag2 Ag 0.45296(12) 0.97871(13) 0.26991(8) 0.0756(7) Uani 0.50 1 d P . . N20 N 0.5640(6) 0.7077(11) 0.3895(4) 0.128(6) Uiso 1 1 d D . . O21 O 0.5321(7) 0.7184(10) 0.4260(5) 0.154 Uiso 1 1 d D . . O22 O 0.6240(6) 0.7110(10) 0.3926(5) 0.154 Uiso 1 1 d D . . O23 O 0.5347(7) 0.6957(10) 0.3476(5) 0.154 Uiso 1 1 d 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 0.0308(4) 0.0174(3) 0.0407(4) -0.0004(3) -0.0080(3) 0.0060(3) Fe1 0.0226(6) 0.0136(6) 0.0320(7) 0.0016(5) -0.0035(5) 0.0040(5) O3 0.017(3) 0.026(3) 0.033(3) 0.002(3) -0.002(2) 0.004(2) O6 0.013(3) 0.015(3) 0.040(3) -0.001(2) -0.005(2) -0.007(2) C30 0.018(4) 0.020(4) 0.027(5) -0.006(3) -0.002(3) 0.001(3) N4 0.044(5) 0.028(4) 0.033(4) 0.004(3) -0.011(3) 0.006(3) O5 0.025(3) 0.008(3) 0.039(3) -0.004(2) -0.002(2) -0.002(2) C1 0.031(5) 0.009(4) 0.041(5) -0.004(3) 0.003(4) 0.003(3) O2 0.020(3) 0.016(3) 0.034(3) -0.002(2) -0.004(2) 0.002(2) N5 0.036(4) 0.024(4) 0.049(5) -0.004(4) 0.000(4) -0.003(3) C9 0.023(4) 0.019(4) 0.042(6) -0.003(4) 0.011(4) 0.000(3) C35 0.019(4) 0.012(4) 0.061(6) -0.007(4) 0.007(4) -0.005(3) N3 0.020(4) 0.041(5) 0.070(6) 0.010(4) -0.001(4) 0.012(4) C29 0.026(5) 0.011(4) 0.047(6) -0.002(4) 0.004(4) 0.000(3) N1 0.049(5) 0.016(4) 0.045(5) 0.001(3) 0.009(4) -0.008(3) C27 0.023(4) 0.011(4) 0.039(5) -0.001(3) -0.002(4) -0.001(3) C13 0.074(8) 0.026(5) 0.058(7) -0.003(5) 0.005(6) -0.007(5) C15 0.036(5) 0.033(5) 0.033(5) 0.006(4) 0.003(4) 0.014(4) N6 0.024(4) 0.022(4) 0.051(5) -0.010(3) 0.002(3) 0.002(3) C14 0.020(4) 0.023(4) 0.036(5) 0.004(4) 0.000(4) 0.004(3) C26 0.038(6) 0.036(6) 0.056(7) 0.007(5) 0.009(5) 0.012(4) C31 0.024(5) 0.015(4) 0.073(7) -0.002(4) 0.007(5) -0.009(3) C17 0.030(5) 0.025(4) 0.043(6) 0.003(4) -0.004(4) 0.007(4) C16 0.031(5) 0.026(4) 0.031(5) 0.011(4) 0.000(4) 0.000(4) C12 0.063(7) 0.028(5) 0.040(6) -0.004(4) 0.015(5) -0.022(5) O4 0.033(3) 0.023(3) 0.030(3) 0.001(3) -0.005(3) 0.008(3) C33 0.023(5) 0.018(4) 0.097(9) -0.017(5) 0.014(5) -0.002(4) C34 0.026(5) 0.020(4) 0.038(5) -0.002(4) 0.004(4) -0.005(3) C32 0.018(4) 0.026(4) 0.034(5) -0.003(4) 0.007(3) -0.003(3) C24 0.021(5) 0.042(6) 0.044(6) 0.007(4) -0.001(4) 0.014(4) C18A 0.062(9) 0.041(7) 0.031(7) -0.006(5) -0.011(6) 0.026(6) C19A 0.052(8) 0.048(7) 0.025(6) -0.004(5) -0.010(5) 0.031(6) C20A 0.051(8) 0.045(7) 0.030(6) -0.003(5) -0.005(5) 0.026(6) C21A 0.070(9) 0.042(7) 0.023(6) -0.006(5) -0.009(6) 0.027(6) C36A 0.025(6) 0.023(6) 0.075(9) -0.001(6) -0.001(6) -0.010(5) C37A 0.026(6) 0.022(6) 0.070(9) 0.004(6) -0.020(6) 0.007(5) C38A 0.027(6) 0.021(5) 0.078(10) -0.006(6) 0.009(6) 0.009(5) C39A 0.014(5) 0.022(6) 0.087(10) 0.016(6) -0.007(6) -0.007(4) C23 0.027(5) 0.037(5) 0.054(6) -0.009(5) -0.009(4) 0.015(4) C28 0.015(4) 0.016(4) 0.060(6) -0.008(4) -0.001(4) 0.001(3) C10 0.044(6) 0.015(4) 0.047(6) -0.001(4) 0.011(5) -0.002(4) C2 0.038(5) 0.009(4) 0.069(7) -0.011(4) -0.020(5) -0.005(4) C25 0.036(6) 0.029(5) 0.067(7) 0.003(5) -0.021(5) 0.014(4) C22 0.020(4) 0.024(4) 0.043(5) 0.007(4) 0.000(4) 0.003(3) C11 0.066(8) 0.023(5) 0.049(7) -0.002(4) -0.010(5) -0.007(5) O1 0.033(3) 0.013(3) 0.035(3) 0.006(2) -0.005(3) 0.008(2) C3 0.062(7) 0.023(5) 0.066(8) -0.008(5) -0.033(6) 0.000(5) Ag2 0.1010(17) 0.0716(13) 0.0476(11) -0.0041(10) -0.0429(11) 0.0055(12) _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 N4 2.276(7) . ? Ag1 N5 2.288(8) . ? Ag1 N6 2.323(7) . ? Ag1 N1 2.367(7) . ? Fe1 O1 1.964(6) . ? Fe1 O5 1.964(6) 2_656 ? Fe1 O3 1.989(6) . ? Fe1 O6 1.989(5) 4_656 ? Fe1 O4 1.997(6) . ? Fe1 O2 2.014(5) . ? O3 C14 1.272(10) . ? O6 C29 1.296(10) . ? O6 Fe1 1.989(5) 4_646 ? C30 C31 1.363(12) . ? C30 C32 1.376(11) . ? C30 C29 1.484(11) . ? N4 C20A 1.305(14) . ? N4 C21A 1.319(13) . ? N4 C21B 1.389(11) . ? N4 C20B 1.394(11) . ? O5 C27 1.282(9) . ? O5 Fe1 1.964(6) 2_656 ? C1 O2 1.260(10) 4_656 ? C1 C2 1.367(13) . ? C1 C9 1.510(11) . ? O2 C1 1.260(10) 4_646 ? N5 C38A 1.329(14) . ? N5 C39A 1.364(13) . ? N5 C39B 1.390(11) . ? N5 C38B 1.391(11) . ? C9 C11 1.371(14) . ? C9 C10 1.378(12) . ? C35 C36A 1.347(14) . ? C35 C37B 1.370(10) . ? C35 C36B 1.373(10) . ? C35 C37A 1.398(14) . ? C35 C27 1.465(12) . ? N3 C26 1.328(14) . ? N3 C25 1.331(14) . ? C29 C28 1.384(12) . ? N1 C12 1.326(13) . ? N1 C13 1.329(13) . ? C27 C28 1.396(11) 3_455 ? C13 C11 1.379(14) . ? C13 H115 0.9300 . ? C15 C14 1.378(12) . ? C15 C16 1.397(12) . ? C15 H116 0.9300 . ? N6 C33 1.335(11) . ? N6 C34 1.346(11) . ? C14 C22 1.518(11) . ? C26 C24 1.414(13) . ? C26 H26 0.9300 . ? C31 C33 1.355(12) . ? C31 H27 0.9300 . ? C17 C19B 1.370(10) . ? C17 C18B 1.372(10) . ? C17 C18A 1.377(14) . ? C17 C19A 1.412(14) . ? C17 C16 1.489(13) . ? C16 O4 1.262(11) . ? C12 C10 1.362(13) . ? C12 H30 0.9300 . ? C33 H34 0.9300 . ? C34 C32 1.384(12) . ? C34 H35 0.9300 . ? C32 H36 0.9300 . ? C24 C22 1.377(13) . ? C24 H37 0.9300 . ? C18A C20A 1.371(16) . ? C18A H58 0.9300 . ? C19A C21A 1.382(15) . ? C19A H32 0.9300 . ? C20A H41 0.9300 . ? C21A H46 0.9300 . ? C21B C19B 1.370(10) . ? C21B H21B 0.9300 . ? C19B H19B 0.9300 . ? C18B C20B 1.372(10) . ? C18B H18B 0.9300 . ? C20B H20B 0.9300 . ? C36A C38A 1.383(16) . ? C36A H54 0.9300 . ? C37A C39A 1.390(15) . ? C37A H24 0.9300 . ? C38A H38 0.9300 . ? C39A H25 0.9300 . ? C36B C38B 1.372(10) . ? C36B H36B 0.9300 . ? C37B C39B 1.370(10) . ? C37B H37B 0.9300 . ? C38B H38B 0.9300 . ? C39B H39B 0.9300 . ? C23 C22 1.382(13) . ? C23 C25 1.393(12) . ? C23 H39 0.9300 . ? C28 C27 1.396(11) 3_545 ? C28 H28 0.9300 . ? C10 H44 0.9300 . ? C2 C3 1.419(14) . ? C2 H45 0.9300 . ? C25 H47 0.9300 . ? C11 H52 0.9300 . ? O1 C3 1.264(10) 4_646 ? C3 O1 1.264(10) 4_656 ? C3 C4B 1.448(13) . ? C3 C4A 1.673(15) . ? N10 O11 1.228(9) 2_655 ? N10 O11 1.228(9) . ? N10 O12 1.236(10) . ? C8A C6A 1.372(8) . ? C8A N2A 1.390(9) . ? C8A H8A 0.9300 . ? C4A C6A 1.354(8) . ? C4A C5A 1.374(8) . ? C5A C7A 1.372(8) . ? C5A H5A 0.9300 . ? C7A N2A 1.397(9) . ? C7A H7A 0.9300 . ? N2A Ag2 2.075(13) 2_655 ? C6A H6A 0.9300 . ? C5B C7B 1.368(8) . ? C5B C4B 1.371(8) . ? C5B H5B 0.9300 . ? C7B N2B 1.391(9) . ? C7B H7B 0.9300 . ? C8B N2B 1.391(9) . ? C8B H8B 0.9300 . ? N2B Ag2 2.114(13) . ? Ag2 N2A 2.075(13) 2_655 ? Ag2 Ag2 2.251(6) 2_655 ? N20 O22 1.220(9) . ? N20 O21 1.220(9) . ? N20 O23 1.247(9) . ? 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 N4 Ag1 N5 132.3(3) . . ? N4 Ag1 N6 104.9(3) . . ? N5 Ag1 N6 105.9(3) . . ? N4 Ag1 N1 103.0(3) . . ? N5 Ag1 N1 95.9(3) . . ? N6 Ag1 N1 115.1(3) . . ? O1 Fe1 O5 97.1(2) . 2_656 ? O1 Fe1 O3 89.5(2) . . ? O5 Fe1 O3 173.0(2) 2_656 . ? O1 Fe1 O6 91.7(2) . 4_656 ? O5 Fe1 O6 87.8(2) 2_656 4_656 ? O3 Fe1 O6 94.5(2) . 4_656 ? O1 Fe1 O4 174.7(2) . . ? O5 Fe1 O4 87.5(2) 2_656 . ? O3 Fe1 O4 85.8(2) . . ? O6 Fe1 O4 91.2(2) 4_656 . ? O1 Fe1 O2 86.7(2) . . ? O5 Fe1 O2 89.9(2) 2_656 . ? O3 Fe1 O2 88.0(2) . . ? O6 Fe1 O2 177.0(2) 4_656 . ? O4 Fe1 O2 90.6(2) . . ? C14 O3 Fe1 121.9(5) . . ? C29 O6 Fe1 125.0(5) . 4_646 ? C31 C30 C32 117.2(7) . . ? C31 C30 C29 121.0(7) . . ? C32 C30 C29 121.8(7) . . ? C20A N4 C21A 116.2(9) . . ? C20A N4 C21B 77.0(18) . . ? C21A N4 C21B 62.8(16) . . ? C20A N4 C20B 67.4(16) . . ? C21A N4 C20B 83.6(17) . . ? C21B N4 C20B 112(3) . . ? C20A N4 Ag1 120.9(7) . . ? C21A N4 Ag1 122.7(7) . . ? C21B N4 Ag1 126(2) . . ? C20B N4 Ag1 122(2) . . ? C27 O5 Fe1 126.9(5) . 2_656 ? O2 C1 C2 125.6(8) 4_656 . ? O2 C1 C9 115.9(8) 4_656 . ? C2 C1 C9 118.5(7) . . ? C1 O2 Fe1 124.0(5) 4_646 . ? C38A N5 C39A 115.4(9) . . ? C38A N5 C39B 60.1(14) . . ? C39A N5 C39B 87.1(15) . . ? C38A N5 C38B 89.0(13) . . ? C39A N5 C38B 63.8(13) . . ? C39B N5 C38B 124(2) . . ? C38A N5 Ag1 120.6(7) . . ? C39A N5 Ag1 123.8(6) . . ? C39B N5 Ag1 117.0(19) . . ? C38B N5 Ag1 119.4(13) . . ? C11 C9 C10 117.9(8) . . ? C11 C9 C1 118.6(8) . . ? C10 C9 C1 123.5(8) . . ? C36A C35 C37B 56.6(13) . . ? C36A C35 C36B 88.9(14) . . ? C37B C35 C36B 112(3) . . ? C36A C35 C37A 119.4(9) . . ? C37B C35 C37A 84.2(15) . . ? C36B C35 C37A 63.5(12) . . ? C36A C35 C27 118.5(8) . . ? C37B C35 C27 125(2) . . ? C36B C35 C27 122.8(16) . . ? C37A C35 C27 121.8(8) . . ? C26 N3 C25 117.3(8) . . ? O6 C29 C28 124.5(7) . . ? O6 C29 C30 114.2(7) . . ? C28 C29 C30 121.2(7) . . ? C12 N1 C13 116.7(9) . . ? C12 N1 Ag1 115.7(6) . . ? C13 N1 Ag1 122.1(7) . . ? O5 C27 C28 122.1(7) . 3_455 ? O5 C27 C35 116.2(7) . . ? C28 C27 C35 121.5(7) 3_455 . ? N1 C13 C11 123.3(11) . . ? N1 C13 H115 118.4 . . ? C11 C13 H115 118.4 . . ? C14 C15 C16 122.1(9) . . ? C14 C15 H116 119.0 . . ? C16 C15 H116 119.0 . . ? C33 N6 C34 115.6(7) . . ? C33 N6 Ag1 123.2(6) . . ? C34 N6 Ag1 115.8(5) . . ? O3 C14 C15 126.0(8) . . ? O3 C14 C22 113.9(7) . . ? C15 C14 C22 120.1(8) . . ? N3 C26 C24 124.1(10) . . ? N3 C26 H26 118.0 . . ? C24 C26 H26 118.0 . . ? C33 C31 C30 120.9(8) . . ? C33 C31 H27 119.5 . . ? C30 C31 H27 119.5 . . ? C19B C17 C18B 123(3) . . ? C19B C17 C18A 83.8(18) . . ? C18B C17 C18A 66.8(16) . . ? C19B C17 C19A 64.9(17) . . ? C18B C17 C19A 85.1(17) . . ? C18A C17 C19A 116.0(9) . . ? C19B C17 C16 119(2) . . ? C18B C17 C16 118(2) . . ? C18A C17 C16 119.4(9) . . ? C19A C17 C16 124.5(8) . . ? O4 C16 C15 124.3(8) . . ? O4 C16 C17 114.2(8) . . ? C15 C16 C17 121.4(9) . . ? N1 C12 C10 124.0(9) . . ? N1 C12 H30 118.0 . . ? C10 C12 H30 118.0 . . ? C16 O4 Fe1 126.3(5) . . ? N6 C33 C31 123.7(9) . . ? N6 C33 H34 118.2 . . ? C31 C33 H34 118.2 . . ? N6 C34 C32 123.6(8) . . ? N6 C34 H35 118.2 . . ? C32 C34 H35 118.2 . . ? C30 C32 C34 119.0(8) . . ? C30 C32 H36 120.5 . . ? C34 C32 H36 120.5 . . ? C22 C24 C26 117.1(9) . . ? C22 C24 H37 121.5 . . ? C26 C24 H37 121.5 . . ? C20A C18A C17 118.9(11) . . ? C20A C18A H58 120.6 . . ? C17 C18A H58 120.6 . . ? C21A C19A C17 119.2(10) . . ? C21A C19A H32 120.4 . . ? C17 C19A H32 120.4 . . ? N4 C20A C18A 125.6(11) . . ? N4 C20A H41 117.2 . . ? C18A C20A H41 117.2 . . ? N4 C21A C19A 123.6(11) . . ? N4 C21A H46 118.2 . . ? C19A C21A H46 118.2 . . ? C19B C21B N4 130(5) . . ? C19B C21B H21B 115.2 . . ? N4 C21B H21B 115.2 . . ? C21B C19B C17 113(4) . . ? C21B C19B H19B 123.3 . . ? C17 C19B H19B 123.3 . . ? C20B C18B C17 119(4) . . ? C20B C18B H18B 120.4 . . ? C17 C18B H18B 120.4 . . ? C18B C20B N4 123(4) . . ? C18B C20B H20B 118.5 . . ? N4 C20B H20B 118.5 . . ? C35 C36A C38A 118.9(10) . . ? C35 C36A H54 120.5 . . ? C38A C36A H54 120.5 . . ? C39A C37A C35 117.0(10) . . ? C39A C37A H24 121.5 . . ? C35 C37A H24 121.5 . . ? N5 C38A C36A 124.5(11) . . ? N5 C38A H38 117.8 . . ? C36A C38A H38 117.8 . . ? N5 C39A C37A 124.0(10) . . ? N5 C39A H25 118.0 . . ? C37A C39A H25 118.0 . . ? C38B C36B C35 127(3) . . ? C38B C36B H36B 116.5 . . ? C35 C36B H36B 116.5 . . ? C39B C37B C35 128(4) . . ? C39B C37B H37B 116.1 . . ? C35 C37B H37B 116.1 . . ? C36B C38B N5 115(3) . . ? C36B C38B H38B 122.6 . . ? N5 C38B H38B 122.6 . . ? C37B C39B N5 114(4) . . ? C37B C39B H39B 122.8 . . ? N5 C39B H39B 122.8 . . ? C22 C23 C25 118.6(9) . . ? C22 C23 H39 120.7 . . ? C25 C23 H39 120.7 . . ? C29 C28 C27 125.3(8) . 3_545 ? C29 C28 H28 117.4 . . ? C27 C28 H28 117.4 3_545 . ? C12 C10 C9 119.1(10) . . ? C12 C10 H44 120.5 . . ? C9 C10 H44 120.5 . . ? C1 C2 C3 123.3(8) . . ? C1 C2 H45 118.3 . . ? C3 C2 H45 118.3 . . ? N3 C25 C23 123.3(10) . . ? N3 C25 H47 118.4 . . ? C23 C25 H47 118.4 . . ? C24 C22 C23 119.6(8) . . ? C24 C22 C14 122.0(8) . . ? C23 C22 C14 118.3(8) . . ? C9 C11 C13 119.0(10) . . ? C9 C11 H52 120.5 . . ? C13 C11 H52 120.5 . . ? C3 O1 Fe1 126.2(7) 4_646 . ? O1 C3 C2 123.7(9) 4_656 . ? O1 C3 C4B 116.5(8) 4_656 . ? C2 C3 C4B 118.6(8) . . ? O1 C3 C4A 118.8(8) 4_656 . ? C2 C3 C4A 114.2(8) . . ? C4B C3 C4A 30.6(4) . . ? O11 N10 O11 124.1(14) 2_655 . ? O11 N10 O12 118.0(7) 2_655 . ? O11 N10 O12 118.0(7) . . ? C6A C8A N2A 121.0(7) . . ? C6A C8A H8A 119.5 . . ? N2A C8A H8A 119.5 . . ? C6A C4A C5A 119.3(5) . . ? C6A C4A C3 107.1(8) . . ? C5A C4A C3 133.6(8) . . ? C7A C5A C4A 120.0(4) . . ? C7A C5A H5A 120.0 . . ? C4A C5A H5A 120.0 . . ? C5A C7A N2A 121.7(7) . . ? C5A C7A H7A 119.2 . . ? N2A C7A H7A 119.2 . . ? C8A N2A C7A 116.6(12) . . ? C8A N2A Ag2 119.2(8) . 2_655 ? C7A N2A Ag2 120.7(9) . 2_655 ? C4A C6A C8A 121.4(4) . . ? C4A C6A H6A 119.3 . . ? C8A C6A H6A 119.3 . . ? C7B C5B C4B 120.1(4) . . ? C7B C5B H5B 120.0 . . ? C4B C5B H5B 120.0 . . ? C5B C4B C3 120.7(8) . . ? C5B C7B N2B 121.7(7) . . ? C5B C7B H7B 119.1 . . ? N2B C7B H7B 119.1 . . ? N2B C8B H8B 118.7 . . ? C8B N2B C7B 116.6(12) . . ? C8B N2B Ag2 123.7(8) . . ? C7B N2B Ag2 119.6(8) . . ? N2A Ag2 N2B 163.3(5) 2_655 . ? N2A Ag2 Ag2 90.8(4) 2_655 2_655 ? N2B Ag2 Ag2 82.9(3) . 2_655 ? O22 N20 O21 121.5(7) . . ? O22 N20 O23 118.9(7) . . ? O21 N20 O23 119.6(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.957 _refine_diff_density_min -1.771 _refine_diff_density_rms 0.177 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.966 -0.004 0.092 1180 436 ' ' 2 0.963 0.002 0.592 1181 436 ' ' # * END # Attachment '- 5_supp780.cif' data_[Fe(III)3L9Ag5](tosilate)5 _database_code_depnum_ccdc_archive 'CCDC 824478' #TrackingRef '- 5_supp780.cif' _chemical_formula_sum 'C152 H116 Ag5 Fe3 N18 O33 S5' _chemical_formula_weight 3589.83 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' _cell_length_a 27.6841(11) _cell_length_b 27.6841(11) _cell_length_c 17.4801(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11602.1(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12741 _cell_measurement_theta_min 2 _cell_measurement_theta_max 19 _exptl_crystal_description hexagonal_prism _exptl_crystal_colour red _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.320 _exptl_crystal_density_diffrn 1.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3622 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ;(Sheldrick G.M.(1996), SADABS University of Gottingen,Germany.) ; _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1 _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_method omega-scan _diffrn_standards_decay_% 0 _diffrn_reflns_number 115880 _diffrn_reflns_av_R_equivalents 0.1072 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 26.44 _reflns_number_total 7950 _reflns_number_gt 3903 _reflns_threshold_expression >2sigma(I) _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics TOPOS _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 crystal is unstable in air, was collected under mineral oil. The structure contains disordered solvents. Because it was difficult to refine a consistent disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. The R before squeeze was: R1 = 0.2140 for 3807 Fo > 4sig(Fo) and 0.2757 for all 7950 data 80 parameters refined using 189 restraints All the light atoms have been refined isotropically. The tosilate anion was refined as rigid model (without hidrogen atoms) and disoreder on the 3-fold axis (33.3%:33.3%:33.3%). Even with such high R value the final model is reliable. The thermal ellipsoids are reasonable and the model chemically meaningful ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7950 _refine_ls_number_parameters 80 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.2368 _refine_ls_R_factor_gt 0.1667 _refine_ls_wR_factor_all 0.4550 _refine_ls_wR_factor_ref 0.4279 _refine_ls_goodness_of_fit_all 1.429 _refine_ls_restrained_S_all 1.413 _refine_ls_shift/su_max 0.003 _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 C1 C 0.6482(7) 0.1000(7) 0.1917(10) 0.123(5) Uiso 1 1 d . . . C2 C 0.6603(7) 0.0907(7) 0.1246(9) 0.127(5) Uiso 1 1 d . . . H2 H 0.6725 0.1208 0.0914 0.152 Uiso 1 1 calc R . . C3 C 0.6587(6) 0.0408(6) 0.0897(11) 0.120(5) Uiso 1 1 d . . . C15 C 0.7118(4) -0.2350(4) -0.2499(6) 0.073(3) Uiso 1 1 d . . . C14 C 0.7669(9) -0.2331(9) -0.2500 0.124(7) Uiso 1 2 d S . . H14 H 0.8005 -0.1995 -0.2500 0.149 Uiso 1 2 calc SR . . C9 C 0.6521(4) 0.1534(3) 0.2122(6) 0.0865(19) Uiso 1 1 d GD . . C10 C 0.6467(4) 0.1593(4) 0.2902(5) 0.142(2) Uiso 1 1 d GD . . H10 H 0.6414 0.1309 0.3237 0.170 Uiso 1 1 calc R . . C12 C 0.6493(5) 0.2075(5) 0.3181(5) 0.166(3) Uiso 1 1 d GD . . H12 H 0.6457 0.2115 0.3703 0.200 Uiso 1 1 calc R . . N1 N 0.6573(4) 0.2499(4) 0.2680(7) 0.138(3) Uiso 1 1 d GD . . C13 C 0.6627(5) 0.2440(4) 0.1900(7) 0.166(3) Uiso 1 1 d GD . . H13 H 0.6680 0.2724 0.1565 0.200 Uiso 1 1 calc R . . C11 C 0.6600(4) 0.1957(4) 0.1621(5) 0.142(2) Uiso 1 1 d GD . . H11 H 0.6636 0.1918 0.1099 0.170 Uiso 1 1 calc R . . C4 C 0.6603(4) 0.0303(4) 0.0147(4) 0.0865(19) Uiso 1 1 d GD . . C6 C 0.6975(4) 0.0727(3) -0.0333(6) 0.142(2) Uiso 1 1 d GD . . H6 H 0.7166 0.1093 -0.0159 0.170 Uiso 1 1 calc R . . C8 C 0.7063(4) 0.0603(4) -0.1073(5) 0.166(3) Uiso 1 1 d GD . . H8 H 0.7312 0.0886 -0.1394 0.200 Uiso 1 1 calc R . . N2 N 0.6778(5) 0.0055(5) -0.1333(4) 0.138(3) Uiso 1 1 d GD . . C7 C 0.6405(5) -0.0369(4) -0.0853(6) 0.166(3) Uiso 1 1 d GD . . H7 H 0.6214 -0.0735 -0.1027 0.200 Uiso 1 1 calc R . . C5 C 0.6318(4) -0.0244(3) -0.0113(5) 0.142(2) Uiso 1 1 d GD . . H5 H 0.6069 -0.0528 0.0208 0.170 Uiso 1 1 calc R . . C16 C 0.7152(4) -0.1796(3) -0.2461(5) 0.0865(19) Uiso 1 1 d GD . . C17 C 0.7593(4) -0.1313(5) -0.2767(7) 0.142(2) Uiso 1 1 d GD . . H17 H 0.7904 -0.1317 -0.2959 0.170 Uiso 1 1 calc R . . C19 C 0.7569(4) -0.0823(4) -0.2784(7) 0.166(3) Uiso 1 1 d GD . . H19 H 0.7864 -0.0500 -0.2988 0.200 Uiso 1 1 calc R . . N3 N 0.7104(5) -0.0817(4) -0.2495(6) 0.138(3) Uiso 1 1 d GD . . C20 C 0.6663(4) -0.1301(5) -0.2190(7) 0.166(3) Uiso 1 1 d GD . . H20 H 0.6352 -0.1296 -0.1997 0.200 Uiso 1 1 calc R . . C18 C 0.6687(4) -0.1790(4) -0.2173(7) 0.142(2) Uiso 1 1 d GD . . H18 H 0.6392 -0.2114 -0.1969 0.170 Uiso 1 1 calc R . . O1 O 0.6318(3) 0.0651(3) 0.2491(5) 0.089(2) Uiso 1 1 d . . . O2 O 0.6379(3) -0.0014(3) 0.1399(4) 0.087(2) Uiso 1 1 d . . . O3 O 0.7225(3) 0.0565(3) 0.2489(5) 0.090(2) Uiso 1 1 d . . . Fe1 Fe 0.64401(8) 0.0000 0.2500 0.0821(8) Uani 1 2 d S . . Ag1 Ag 0.6667 0.3333 0.30205(8) 0.0789(6) Uani 1 3 d S . . Ag2 Ag 0.70832(5) 0.0000 -0.2500 0.0883(6) Uani 1 2 d S . . S100 S 0.6667 0.3333 0.4922(4) 0.0195(14) Uiso 0.33 3 d SPG . . C101 C 0.6289(2) 0.257371(9) 0.4956(4) 0.037(4) Uiso 0.33 1 d PG . . C102 C 0.5760(3) 0.22997(17) 0.4638(9) 0.080(9) Uiso 0.33 1 d PG . . C103 C 0.6526(4) 0.22723(17) 0.5249(9) 0.071(8) Uiso 0.33 1 d PG . . C104 C 0.5465(4) 0.17214(17) 0.4609(10) 0.082(9) Uiso 0.33 1 d PG . . C105 C 0.6226(6) 0.16931(16) 0.5209(10) 0.074(8) Uiso 0.33 1 d PG . . C106 C 0.5696(5) 0.141063(9) 0.4892(9) 0.077(9) Uiso 0.33 1 d PG . . C107 C 0.5379(7) 0.078516(18) 0.4859(12) 0.108(12) Uiso 0.33 1 d PG . . O101 O 0.7013(5) 0.3441(2) 0.4228(7) 0.256(19) Uiso 0.33 1 d PG . . O102 O 0.62869(14) 0.35062(17) 0.4913(10) 0.256(19) Uiso 0.33 1 d PG . . O103 O 0.7026(5) 0.3485(2) 0.5616(7) 0.256(19) Uiso 0.33 1 d PG . . 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 Fe1 0.0877(13) 0.0468(11) 0.0981(17) 0.0096(10) 0.0048(5) 0.0234(6) Ag1 0.0879(8) 0.0879(8) 0.0609(9) 0.000 0.000 0.0440(4) Ag2 0.1017(8) 0.0723(8) 0.0810(9) -0.0141(6) -0.0071(3) 0.0362(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 C1 C2 1.282(19) . ? C1 O1 1.306(16) . ? C1 C9 1.470(17) . ? C2 C3 1.49(2) . ? C2 H2 0.9300 . ? C3 C4 1.349(19) . ? C3 O2 1.339(17) . ? C15 O3 1.224(11) 9_545 ? C15 C14 1.498(15) . ? C15 C16 1.491(13) . ? C14 C15 1.498(15) 6_644 ? C14 H14 0.9300 . ? C9 C10 1.3900 . ? C9 C11 1.3900 . ? C10 C12 1.3900 . ? C10 H10 0.9300 . ? C12 N1 1.3900 . ? C12 H12 0.9300 . ? N1 C13 1.3900 . ? N1 Ag1 2.271(7) . ? C13 C11 1.3900 . ? C13 H13 0.9300 . ? C11 H11 0.9300 . ? C4 C6 1.3900 . ? C4 C5 1.3900 . ? C6 C8 1.3900 . ? C6 H6 0.9300 . ? C8 N2 1.3900 . ? C8 H8 0.9300 . ? N2 C7 1.3900 . ? N2 Ag2 2.243(7) . ? C7 C5 1.3900 . ? C7 H7 0.9300 . ? C5 H5 0.9300 . ? C16 C17 1.3900 . ? C16 C18 1.3900 . ? C17 C19 1.3900 . ? C17 H17 0.9300 . ? C19 N3 1.3900 . ? C19 H19 0.9300 . ? N3 C20 1.3900 . ? N3 Ag2 2.292(8) . ? C20 C18 1.3900 . ? C20 H20 0.9300 . ? C18 H18 0.9300 . ? O1 Fe1 1.994(8) . ? O2 Fe1 1.931(7) . ? O3 C15 1.224(11) 8_665 ? O3 Fe1 1.943(8) . ? Fe1 O2 1.931(7) 4 ? Fe1 O3 1.943(8) 4 ? Fe1 O1 1.994(8) 4 ? Ag1 O101 2.275(16) . ? Ag1 O101 2.275(7) 3_665 ? Ag1 O101 2.275(8) 2_655 ? Ag1 N1 2.271(13) 3_665 ? Ag1 N1 2.271(13) 2_655 ? Ag2 N2 2.243(13) 4_554 ? Ag2 N3 2.292(14) 4_554 ? S100 O102 1.356(4) 2_655 ? S100 O102 1.356(4) 3_665 ? S100 O102 1.3555 . ? S100 O101 1.482(10) 3_665 ? S100 O101 1.482(14) 2_655 ? S100 O101 1.4818 . ? S100 O103 1.490(9) 3_665 ? S100 O103 1.4902 . ? S100 O103 1.490(15) 2_655 ? S100 C101 1.8222 . ? S100 C101 1.822(5) 2_655 ? S100 C101 1.822(5) 3_665 ? C101 O102 0.5747(15) 2_655 ? C101 C102 1.3849 . ? C101 C103 1.3900 . ? C101 O103 1.504(8) 3_665 ? C101 O101 1.625(7) 3_665 ? C102 C104 1.3875 . ? C102 O102 1.850(4) 2_655 ? C103 C105 1.3908 . ? C103 O102 1.568(5) 2_655 ? C104 C106 1.3941 . ? C105 C106 1.3875 . ? C106 C107 1.5008 . ? O101 O102 1.3778 3_665 ? O101 O101 1.47(2) 2_655 ? O101 O101 1.47(2) 3_665 ? O101 C101 1.625(4) 2_655 ? O102 C101 0.575(9) 3_665 ? O102 O103 1.364(9) 2_655 ? O102 O101 1.378(10) 2_655 ? O102 C103 1.568(11) 3_665 ? O102 C102 1.850(13) 3_665 ? O103 O102 1.3637 3_665 ? O103 C101 1.504(4) 2_655 ? O103 O103 1.50(2) 3_665 ? O103 O103 1.50(2) 2_655 ? 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 C2 C1 O1 125.6(16) . . ? C2 C1 C9 122.1(16) . . ? O1 C1 C9 112.3(13) . . ? C1 C2 C3 132.3(17) . . ? C1 C2 H2 113.9 . . ? C3 C2 H2 113.9 . . ? C4 C3 O2 119.7(13) . . ? C4 C3 C2 127.4(15) . . ? O2 C3 C2 110.0(14) . . ? O3 C15 C14 125.5(12) 9_545 . ? O3 C15 C16 119.2(9) 9_545 . ? C14 C15 C16 115.1(11) . . ? C15 C14 C15 116.5(17) . 6_644 ? C15 C14 H14 121.7 . . ? C15 C14 H14 121.7 6_644 . ? C10 C9 C11 120.0 . . ? C10 C9 C1 113.5(10) . . ? C11 C9 C1 126.5(10) . . ? C12 C10 C9 120.0 . . ? C12 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C12 N1 120.0 . . ? C10 C12 H12 120.0 . . ? N1 C12 H12 120.0 . . ? C13 N1 C12 120.0 . . ? C13 N1 Ag1 114.3(7) . . ? C12 N1 Ag1 125.6(7) . . ? N1 C13 C11 120.0 . . ? N1 C13 H13 120.0 . . ? C11 C13 H13 120.0 . . ? C13 C11 C9 120.0 . . ? C13 C11 H11 120.0 . . ? C9 C11 H11 120.0 . . ? C3 C4 C6 119.8(10) . . ? C3 C4 C5 119.3(10) . . ? C6 C4 C5 120.0 . . ? C4 C6 C8 120.0 . . ? C4 C6 H6 120.0 . . ? C8 C6 H6 120.0 . . ? N2 C8 C6 120.0 . . ? N2 C8 H8 120.0 . . ? C6 C8 H8 120.0 . . ? C8 N2 C7 120.0 . . ? C8 N2 Ag2 110.1(6) . . ? C7 N2 Ag2 129.6(6) . . ? C5 C7 N2 120.0 . . ? C5 C7 H7 120.0 . . ? N2 C7 H7 120.0 . . ? C7 C5 C4 120.0 . . ? C7 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C17 C16 C18 120.0 . . ? C17 C16 C15 123.1(8) . . ? C18 C16 C15 116.5(8) . . ? C16 C17 C19 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C17 H17 120.0 . . ? N3 C19 C17 120.0 . . ? N3 C19 H19 120.0 . . ? C17 C19 H19 120.0 . . ? C19 N3 C20 120.0 . . ? C19 N3 Ag2 119.4(6) . . ? C20 N3 Ag2 120.6(6) . . ? N3 C20 C18 120.0 . . ? N3 C20 H20 120.0 . . ? C18 C20 H20 120.0 . . ? C20 C18 C16 120.0 . . ? C20 C18 H18 120.0 . . ? C16 C18 H18 120.0 . . ? C1 O1 Fe1 121.4(9) . . ? C3 O2 Fe1 129.8(9) . . ? C15 O3 Fe1 131.9(7) 8_665 . ? O2 Fe1 O2 171.2(4) . 4 ? O2 Fe1 O3 93.0(3) . 4 ? O2 Fe1 O3 93.3(3) 4 4 ? O2 Fe1 O3 93.3(3) . . ? O2 Fe1 O3 93.0(3) 4 . ? O3 Fe1 O3 88.5(5) 4 . ? O2 Fe1 O1 87.6(3) . . ? O2 Fe1 O1 86.9(3) 4 . ? O3 Fe1 O1 172.7(3) 4 . ? O3 Fe1 O1 84.2(3) . . ? O2 Fe1 O1 86.9(3) . 4 ? O2 Fe1 O1 87.6(3) 4 4 ? O3 Fe1 O1 84.2(3) 4 4 ? O3 Fe1 O1 172.7(3) . 4 ? O1 Fe1 O1 103.1(5) . 4 ? O101 Ag1 O101 37.7(5) . 3_665 ? O101 Ag1 O101 37.7(6) . 2_655 ? O101 Ag1 N1 125.0(9) . 3_665 ? O101 Ag1 N1 101.7(8) 3_665 3_665 ? O101 Ag1 N1 87.3(9) 2_655 3_665 ? O101 Ag1 N1 87.3(9) . 2_655 ? O101 Ag1 N1 125.0(9) 3_665 2_655 ? O101 Ag1 N1 101.7(9) 2_655 2_655 ? N1 Ag1 N1 113.4(7) 3_665 2_655 ? O101 Ag1 N1 101.7(4) . . ? O101 Ag1 N1 87.3(4) 3_665 . ? O101 Ag1 N1 125.0(5) 2_655 . ? N1 Ag1 N1 113.4(7) 3_665 . ? N1 Ag1 N1 113.4(6) 2_655 . ? N2 Ag2 N2 131.5(10) . 4_554 ? N2 Ag2 N3 99.6(8) . 4_554 ? N2 Ag2 N3 105.1(12) 4_554 4_554 ? N2 Ag2 N3 105.1(4) . . ? N2 Ag2 N3 99.6(9) 4_554 . ? N3 Ag2 N3 117.5(10) 4_554 . ? O102 S100 O102 120.0 2_655 3_665 ? O102 S100 O102 120.0(3) 2_655 . ? O102 S100 O102 120.0(3) 3_665 . ? O102 S100 O101 57.9(3) 2_655 3_665 ? O102 S100 O101 117.2(9) 3_665 3_665 ? O102 S100 O101 92.5(7) . 3_665 ? O102 S100 O101 117.2(5) 2_655 2_655 ? O102 S100 O101 92.5(4) 3_665 2_655 ? O102 S100 O101 57.9(8) . 2_655 ? O101 S100 O101 59.5(5) 3_665 2_655 ? O102 S100 O101 92.52(16) 2_655 . ? O102 S100 O101 57.90(8) 3_665 . ? O102 S100 O101 117.2 . . ? O101 S100 O101 59.5(9) 3_665 . ? O101 S100 O101 59.5(8) 2_655 . ? O102 S100 O103 57.0(3) 2_655 3_665 ? O102 S100 O103 115.9(9) 3_665 3_665 ? O102 S100 O103 97.9(8) . 3_665 ? O101 S100 O103 109.70(16) 3_665 3_665 ? O101 S100 O103 150.3(6) 2_655 3_665 ? O101 S100 O103 142.7(5) . 3_665 ? O102 S100 O103 97.93(16) 2_655 . ? O102 S100 O103 57.03(6) 3_665 . ? O102 S100 O103 115.9 . . ? O101 S100 O103 150.3(6) 3_665 . ? O101 S100 O103 142.7(4) 2_655 . ? O101 S100 O103 109.7 . . ? O103 S100 O103 60.4(8) 3_665 . ? O102 S100 O103 115.9(5) 2_655 2_655 ? O102 S100 O103 97.9(4) 3_665 2_655 ? O102 S100 O103 57.0(8) . 2_655 ? O101 S100 O103 142.7(6) 3_665 2_655 ? O101 S100 O103 109.70(15) 2_655 2_655 ? O101 S100 O103 150.3(4) . 2_655 ? O103 S100 O103 60.4(5) 3_665 2_655 ? O103 S100 O103 60.4(7) . 2_655 ? O102 S100 C101 12.3(3) 2_655 . ? O102 S100 C101 132.0(3) 3_665 . ? O102 S100 C101 108.0 . . ? O101 S100 C101 57.8(4) 3_665 . ? O101 S100 C101 114.5(4) 2_655 . ? O101 S100 C101 101.4 . . ? O103 S100 C101 52.8(4) 3_665 . ? O103 S100 C101 102.5 . . ? O103 S100 C101 108.0(4) 2_655 . ? O102 S100 C101 108.0 2_655 2_655 ? O102 S100 C101 12.3 3_665 2_655 ? O102 S100 C101 132.0(3) . 2_655 ? O101 S100 C101 114.5(9) 3_665 2_655 ? O101 S100 C101 101.4(5) 2_655 2_655 ? O101 S100 C101 57.8 . 2_655 ? O103 S100 C101 108.0(9) 3_665 2_655 ? O103 S100 C101 52.8 . 2_655 ? O103 S100 C101 102.5(5) 2_655 2_655 ? C101 S100 C101 119.9(3) . 2_655 ? O102 S100 C101 132.0 2_655 3_665 ? O102 S100 C101 108.0 3_665 3_665 ? O102 S100 C101 12.3(3) . 3_665 ? O101 S100 C101 101.4(6) 3_665 3_665 ? O101 S100 C101 57.8(8) 2_655 3_665 ? O103 S100 C101 102.5(6) 3_665 3_665 ? O103 S100 C101 52.8(8) 2_655 3_665 ? C101 S100 C101 119.9(3) . 3_665 ? C101 S100 C101 119.9 2_655 3_665 ? O102 C101 C102 137.6(5) 2_655 . ? O102 C101 C103 97.0(7) 2_655 . ? C102 C101 C103 120.3 . . ? O102 C101 O103 65.0(8) 2_655 3_665 ? C102 C101 O103 124.6(9) . 3_665 ? C103 C101 O103 95.3(5) . 3_665 ? O102 C101 O101 55.0(8) 2_655 3_665 ? C102 C101 O101 83.3(9) . 3_665 ? C103 C101 O101 134.1(7) . 3_665 ? O103 C101 O101 101.87(7) 3_665 3_665 ? O102 C101 S100 30.0(7) 2_655 . ? C102 C101 S100 117.3 . . ? C103 C101 S100 122.3 . . ? O103 C101 S100 52.2(5) 3_665 . ? O101 C101 S100 50.5(5) 3_665 . ? C101 C102 C104 119.9 . . ? C101 C102 O102 12.10(11) . 2_655 ? C101 C103 C105 119.1 . . ? C101 C103 O102 21.34(17) . 2_655 ? C102 C104 C106 120.8 . . ? C106 C105 C103 121.5 . . ? C105 C106 C104 118.4 . . ? C105 C106 C107 120.6 . . ? C104 C106 C107 120.9 . . ? O102 O101 O101 92.1(3) 3_665 2_655 ? O102 O101 O101 116.46(17) 3_665 3_665 ? O101 O101 O101 60.0 2_655 3_665 ? O102 O101 S100 56.45(18) 3_665 . ? O101 O101 S100 60.25(14) 2_655 . ? O101 O101 S100 60.24(14) 3_665 . ? O102 O101 C101 20.0(2) 3_665 2_655 ? O101 O101 C101 111.9(2) 2_655 2_655 ? O101 O101 C101 128.1(2) 3_665 2_655 ? S100 O101 C101 71.66(12) . 2_655 ? O102 O101 Ag1 155.5(6) 3_665 . ? O101 O101 Ag1 71.1(9) 2_655 . ? O101 O101 Ag1 71.1(7) 3_665 . ? S100 O101 Ag1 123.1(9) . . ? C101 O101 Ag1 160.1(6) 2_655 . ? C101 O102 O103 92.6(9) 3_665 2_655 ? C101 O102 S100 137.7(5) 3_665 . ? O103 O102 S100 66.5(10) 2_655 . ? C101 O102 O101 105.0(10) 3_665 2_655 ? O103 O102 O101 124.8(4) 2_655 2_655 ? S100 O102 O101 65.7(10) . 2_655 ? C101 O102 C103 61.62(15) 3_665 3_665 ? O103 O102 C103 93.5(7) 2_655 3_665 ? S100 O102 C103 149.5(4) . 3_665 ? O101 O102 C103 141.0(7) 2_655 3_665 ? C101 O102 C102 30.3(4) 3_665 3_665 ? O103 O102 C102 104.4(9) 2_655 3_665 ? S100 O102 C102 117.2(4) . 3_665 ? O101 O102 C102 75.4(7) 2_655 3_665 ? C103 O102 C102 89.1(5) 3_665 3_665 ? O102 O103 S100 56.51(17) 3_665 . ? O102 O103 C101 22.5(2) 3_665 2_655 ? S100 O103 C101 74.99(14) . 2_655 ? O102 O103 O103 114.84(10) 3_665 3_665 ? S100 O103 O103 59.81(17) . 3_665 ? C101 O103 O103 127.0(3) 2_655 3_665 ? O102 O103 O103 97.2(3) 3_665 2_655 ? S100 O103 O103 59.81(17) . 2_655 ? C101 O103 O103 119.3(3) 2_655 2_655 ? O103 O103 O103 60.0 3_665 2_655 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 5.351 _refine_diff_density_min -1.150 _refine_diff_density_rms 0.222 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 5775 3089 ' ' # * END