# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Chun-ying Duan' _publ_contact_author_address ; State Key Laboratory Coordination Chemistry Institute Nanjing University Nanjing 210093 CHINA ; _publ_contact_author_email DUANCY@NJU.EDU.CN _publ_section_title ; Spontaneous resolution of silver double helicates consisting of achiral ligands with several aromatic rings ; loop_ _publ_author_name 'Chun-ying Duan' 'Bai Yan' 'He Guangjie' 'Lin Zhi-hua' 'Meng Qing-jin' ; Sun Qiazhen ; # Attachment 'compound 2-M.txt' data_compound_2-M _database_code_depnum_ccdc_archive 'CCDC 262384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 Ag2 Cl1.67 N12.33 O7.67' _chemical_formula_weight 1235.12 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 15.2573(9) _cell_length_b 15.2573(9) _cell_length_c 21.4188(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4318.0(5) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1358 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 13.89 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1866 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 21618 _diffrn_reflns_av_R_equivalents 0.1060 _diffrn_reflns_av_sigmaI/netI 0.1553 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5058 _reflns_number_gt 2043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(5) _refine_ls_number_reflns 5058 _refine_ls_number_parameters 347 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1639 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.092 _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 0.48102(7) 0.36108(6) 0.54573(4) 0.0918(3) Uani 1 1 d . . . N1 N 0.3477(8) 0.2176(8) 0.5677(6) 0.088(3) Uani 1 1 d . . . N2 N 0.3995(7) 0.2862(8) 0.4449(5) 0.079(3) Uani 1 1 d . . . N3 N 0.4055(7) 0.3084(7) 0.3791(4) 0.067(3) Uani 1 1 d . . . N4 N 0.6056(7) 0.5223(8) 0.4311(4) 0.067(3) Uani 1 1 d . . . N5 N 0.5376(7) 0.5513(7) 0.4278(4) 0.068(3) Uani 1 1 d . . . N6 N 0.4120(9) 0.6425(8) 0.4352(4) 0.088(4) Uani 1 1 d . . . C1 C 0.3118(13) 0.1806(12) 0.6241(8) 0.107(6) Uani 1 1 d . . . H1A H 0.3460 0.2250 0.6567 0.128 Uiso 1 1 calc R . . C2 C 0.2385(19) 0.0948(19) 0.6414(10) 0.170(10) Uani 1 1 d . . . H2A H 0.2274 0.0748 0.6830 0.204 Uiso 1 1 calc R . . C3 C 0.1815(14) 0.0382(14) 0.5972(10) 0.186(11) Uani 1 1 d . . . H3A H 0.1255 -0.0242 0.6068 0.224 Uiso 1 1 calc R . . C4 C 0.2021(12) 0.0685(12) 0.5359(8) 0.153(7) Uani 1 1 d . . . H4A H 0.1589 0.0291 0.5040 0.183 Uiso 1 1 calc R . . C5 C 0.2910(10) 0.1618(11) 0.5226(7) 0.082(4) Uani 1 1 d . . . C6 C 0.3211(10) 0.2024(11) 0.4586(7) 0.082(4) Uani 1 1 d . . . H6A H 0.2795 0.1639 0.4259 0.099 Uiso 1 1 calc R . . C7 C 0.4901(9) 0.3776(9) 0.3635(5) 0.062(3) Uani 1 1 d . . . C8 C 0.5039(11) 0.4047(10) 0.2956(5) 0.069(3) Uani 1 1 d . . . C9 C 0.5860(10) 0.4924(10) 0.2732(6) 0.076(4) Uani 1 1 d . . . H9A H 0.6347 0.5374 0.3009 0.092 Uiso 1 1 calc R . . C10 C 0.5962(11) 0.5135(10) 0.2110(7) 0.100(5) Uani 1 1 d . . . H10A H 0.6498 0.5740 0.1964 0.120 Uiso 1 1 calc R . . C11 C 0.5308(12) 0.4488(13) 0.1724(6) 0.100(5) Uani 1 1 d . . . H11A H 0.5409 0.4621 0.1298 0.120 Uiso 1 1 calc R . . C12 C 0.4489(10) 0.3633(11) 0.1912(7) 0.104(5) Uani 1 1 d . . . H12A H 0.4011 0.3204 0.1624 0.125 Uiso 1 1 calc R . . C13 C 0.4361(9) 0.3391(9) 0.2553(6) 0.096(4) Uani 1 1 d . . . H13A H 0.3815 0.2787 0.2692 0.116 Uiso 1 1 calc R . . C14 C 0.5785(10) 0.4333(10) 0.4030(5) 0.062(3) Uani 1 1 d . . . C15 C 0.6533(9) 0.3987(12) 0.4049(4) 0.067(3) Uani 1 1 d . . . C16 C 0.7597(11) 0.4692(9) 0.4158(4) 0.081(4) Uani 1 1 d . . . H16A H 0.7834 0.5375 0.4233 0.098 Uiso 1 1 calc R . . C17 C 0.8242(10) 0.4302(13) 0.4146(6) 0.091(5) Uani 1 1 d . . . H17A H 0.8929 0.4743 0.4211 0.109 Uiso 1 1 calc R . . C18 C 0.7939(13) 0.3353(14) 0.4048(6) 0.093(5) Uani 1 1 d . . . H18A H 0.8404 0.3128 0.4045 0.111 Uiso 1 1 calc R . . C19 C 0.6972(14) 0.2709(12) 0.3953(5) 0.097(5) Uani 1 1 d . . . H19A H 0.6783 0.2037 0.3880 0.116 Uiso 1 1 calc R . . C20 C 0.6208(9) 0.2960(11) 0.3954(5) 0.074(4) Uani 1 1 d . . . H20A H 0.5530 0.2479 0.3896 0.089 Uiso 1 1 calc R . . C21 C 0.5787(9) 0.6489(11) 0.4258(5) 0.080(4) Uani 1 1 d . . . H21A H 0.6488 0.6893 0.4240 0.096 Uiso 1 1 calc R . . C22 C 0.5125(17) 0.6981(12) 0.4266(5) 0.092(5) Uani 1 1 d . . . C23 C 0.5699(10) 0.8102(11) 0.4174(5) 0.078(3) Uani 1 1 d . . . H23A H 0.6399 0.8452 0.4127 0.093 Uiso 1 1 calc R . . C24 C 0.5175(14) 0.8575(12) 0.4162(6) 0.104(5) Uani 1 1 d . . . H24A H 0.5490 0.9273 0.4109 0.125 Uiso 1 1 calc R . . C25 C 0.4154(16) 0.8001(16) 0.4229(6) 0.117(6) Uani 1 1 d . . . H25A H 0.3777 0.8324 0.4193 0.141 Uiso 1 1 calc R . . C26 C 0.3615(11) 0.6929(11) 0.4352(5) 0.079(4) Uani 1 1 d . . . H26A H 0.2923 0.6593 0.4430 0.095 Uiso 1 1 calc R . . Cl1 Cl 0.3628(3) 0.0000 0.3333 0.1195(18) Uani 1 2 d SDU . . O1 O 0.4594(6) 0.0000 0.3333 0.189(6) Uiso 1 2 d SDU . . O2 O 0.3729(11) 0.0930(9) 0.3174(10) 0.125(6) Uiso 0.50 1 d PDU . . O3 O 0.3155(13) -0.0718(15) 0.2828(9) 0.199(8) Uiso 0.50 1 d PDU . . O4 O 0.3093(13) -0.0428(17) 0.3887(7) 0.164(7) Uiso 0.50 1 d PDU . . Cl2 Cl 0.8306(8) 0.9095(7) 0.5093(4) 0.170(5) Uiso 0.33 1 d PDU A 1 O6 O 0.9217(14) 0.931(2) 0.5397(10) 0.197(11) Uiso 0.33 1 d PDU A 1 O7 O 0.8284(18) 0.8760(17) 0.4475(7) 0.165(10) Uiso 0.33 1 d PDU A 1 O8 O 0.822(2) 0.9990(14) 0.5081(11) 0.235(13) Uiso 0.33 1 d PDU A 1 O9 O 0.7458(16) 0.8338(17) 0.5440(10) 0.223(14) Uiso 0.33 1 d PDU A 1 N7 N 0.8306(8) 0.9095(7) 0.5093(4) 0.170(5) Uiso 0.17 1 d PDU B 2 O7' O 0.762(3) 0.910(3) 0.543(2) 0.182(17) Uiso 0.17 1 d PDU B 2 O6' O 0.8266(15) 0.8266(15) 0.5000 0.157(11) Uiso 0.33 2 d SPDU B 2 O8' O 0.9192(16) 0.977(3) 0.526(3) 0.23(2) Uiso 0.17 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0753(7) 0.0746(7) 0.1041(6) -0.0104(6) -0.0035(6) 0.0215(6) N1 0.110(10) 0.107(10) 0.060(7) 0.006(8) -0.005(7) 0.064(8) N2 0.061(7) 0.050(7) 0.096(8) 0.013(6) 0.001(6) 0.006(6) N3 0.057(7) 0.074(8) 0.064(6) -0.003(6) -0.013(5) 0.028(6) N4 0.065(7) 0.088(9) 0.080(8) 0.008(6) -0.018(6) 0.061(7) N5 0.077(8) 0.049(7) 0.069(6) 0.007(6) 0.012(5) 0.024(7) N6 0.041(7) 0.117(10) 0.074(7) -0.001(6) 0.009(6) 0.015(8) C1 0.104(14) 0.081(12) 0.106(14) 0.020(10) 0.016(11) 0.024(10) C2 0.16(2) 0.20(3) 0.127(17) -0.022(19) -0.044(16) 0.08(2) C3 0.117(17) 0.17(2) 0.19(2) 0.159(19) 0.057(16) 0.009(14) C4 0.099(14) 0.102(13) 0.159(16) 0.010(12) -0.048(12) -0.023(11) C5 0.058(10) 0.078(11) 0.086(11) 0.019(9) -0.009(9) 0.015(9) C6 0.076(10) 0.084(11) 0.109(12) -0.030(9) -0.046(9) 0.057(9) C7 0.029(7) 0.066(9) 0.079(9) -0.015(7) 0.009(7) 0.015(8) C8 0.096(11) 0.104(11) 0.047(8) -0.006(8) -0.002(8) 0.080(10) C9 0.083(11) 0.102(11) 0.051(9) 0.013(8) 0.003(7) 0.051(10) C10 0.079(11) 0.098(12) 0.107(13) 0.044(10) -0.015(10) 0.032(10) C11 0.071(12) 0.167(17) 0.081(10) 0.027(11) 0.016(10) 0.074(12) C12 0.079(11) 0.122(14) 0.092(11) -0.049(9) -0.031(9) 0.036(11) C13 0.106(11) 0.103(11) 0.061(8) -0.033(9) -0.029(8) 0.038(9) C14 0.082(10) 0.069(10) 0.049(7) 0.018(7) 0.017(7) 0.048(9) C15 0.066(9) 0.095(11) 0.051(7) 0.010(7) 0.006(6) 0.050(10) C16 0.102(11) 0.064(9) 0.065(8) -0.015(7) 0.004(8) 0.032(10) C17 0.074(11) 0.136(14) 0.088(10) 0.019(10) 0.015(8) 0.071(12) C18 0.090(13) 0.142(16) 0.067(9) 0.007(11) 0.018(10) 0.073(14) C19 0.147(15) 0.122(15) 0.066(9) 0.027(9) 0.023(10) 0.102(14) C20 0.088(11) 0.093(11) 0.073(8) -0.011(8) -0.002(7) 0.069(10) C21 0.073(10) 0.106(12) 0.062(8) -0.012(8) -0.018(7) 0.046(10) C22 0.198(17) 0.088(12) 0.044(8) -0.009(8) -0.032(10) 0.114(13) C23 0.065(9) 0.079(12) 0.078(8) -0.004(8) -0.005(7) 0.028(8) C24 0.108(14) 0.100(15) 0.102(9) -0.021(9) -0.005(11) 0.051(12) C25 0.21(2) 0.158(19) 0.073(9) -0.011(11) -0.027(12) 0.154(17) C26 0.104(12) 0.096(12) 0.067(8) 0.003(8) -0.016(8) 0.072(11) Cl1 0.131(3) 0.106(4) 0.114(4) 0.021(3) 0.0107(17) 0.053(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.167(11) . ? Ag1 N6 2.219(12) 4_556 ? Ag1 N5 2.415(10) 4_556 ? Ag1 N2 2.469(9) . ? N1 C5 1.292(13) . ? N1 C1 1.330(15) . ? N2 C6 1.273(13) . ? N2 N3 1.442(10) . ? N3 C7 1.236(10) . ? N4 N5 1.319(11) . ? N4 C14 1.347(12) . ? N5 C21 1.296(13) . ? N5 Ag1 2.415(10) 4_556 ? N6 C26 1.334(14) . ? N6 C22 1.344(18) . ? N6 Ag1 2.219(12) 4_556 ? C1 C2 1.28(2) . ? C1 H1A 0.9300 . ? C2 C3 1.28(2) . ? C2 H2A 0.9300 . ? C3 C4 1.376(19) . ? C3 H3A 0.9300 . ? C4 C5 1.420(17) . ? C4 H4A 0.9300 . ? C5 C6 1.481(16) . ? C6 H6A 0.9300 . ? C7 C14 1.452(14) . ? C7 C8 1.499(12) . ? C8 C13 1.335(12) . ? C8 C9 1.383(13) . ? C9 C10 1.361(14) . ? C9 H9A 0.9300 . ? C10 C11 1.291(14) . ? C10 H10A 0.9300 . ? C11 C12 1.340(14) . ? C11 H11A 0.9300 . ? C12 C13 1.409(13) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.479(13) . ? C15 C20 1.401(14) . ? C15 C16 1.450(14) . ? C16 C17 1.381(15) . ? C16 H16A 0.9300 . ? C17 C18 1.298(16) . ? C17 H17A 0.9300 . ? C18 C19 1.317(16) . ? C18 H18A 0.9300 . ? C19 C20 1.397(15) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.530(16) . ? C21 H21A 0.9300 . ? C22 C23 1.493(17) . ? C23 C24 1.319(15) . ? C23 H23A 0.9300 . ? C24 C25 1.359(17) . ? C24 H24A 0.9300 . ? C25 C26 1.440(19) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? Cl1 O2 1.391(8) . ? Cl1 O2 1.391(8) 5 ? Cl1 O4 1.402(9) 5 ? Cl1 O4 1.402(9) . ? Cl1 O3 1.450(9) . ? Cl1 O3 1.450(9) 5 ? Cl1 O1 1.474(8) . ? O2 O4 1.076(18) 5 ? O2 O3 1.501(18) 5 ? O3 O2 1.501(18) 5 ? O3 O4 1.549(19) 5 ? O4 O2 1.076(18) 5 ? O4 O3 1.549(19) 5 ? Cl2 O7 1.414(10) . ? Cl2 O6 1.417(10) . ? Cl2 O9 1.438(10) . ? Cl2 O8 1.440(10) . ? Cl2 O6 1.79(3) 4_556 ? Cl2 O7 1.93(3) 4_556 ? Cl2 Cl2 2.123(19) 4_556 ? O6 O7 1.38(3) 4_556 ? O6 O6 1.72(5) 4_556 ? O6 Cl2 1.79(3) 4_556 ? O7 O6 1.38(3) 4_556 ? O7 Cl2 1.93(3) 4_556 ? O6' N7 1.252(10) 4_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N6 129.1(4) . 4_556 ? N1 Ag1 N5 138.1(4) . 4_556 ? N6 Ag1 N5 76.7(4) 4_556 4_556 ? N1 Ag1 N2 73.8(4) . . ? N6 Ag1 N2 122.5(3) 4_556 . ? N5 Ag1 N2 124.2(3) 4_556 . ? C5 N1 C1 113.6(13) . . ? C5 N1 Ag1 119.0(9) . . ? C1 N1 Ag1 127.2(11) . . ? C6 N2 N3 112.2(10) . . ? C6 N2 Ag1 105.5(8) . . ? N3 N2 Ag1 142.0(7) . . ? C7 N3 N2 112.4(9) . . ? N5 N4 C14 114.7(10) . . ? C21 N5 N4 112.1(10) . . ? C21 N5 Ag1 108.1(8) . 4_556 ? N4 N5 Ag1 136.8(8) . 4_556 ? C26 N6 C22 116.2(12) . . ? C26 N6 Ag1 131.2(10) . 4_556 ? C22 N6 Ag1 112.5(10) . 4_556 ? C2 C1 N1 131(2) . . ? C2 C1 H1A 114.3 . . ? N1 C1 H1A 114.3 . . ? C1 C2 C3 115(2) . . ? C1 C2 H2A 122.4 . . ? C3 C2 H2A 122.4 . . ? C2 C3 C4 120.9(19) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C3 C4 C5 118.1(15) . . ? C3 C4 H4A 120.9 . . ? C5 C4 H4A 120.9 . . ? N1 C5 C4 120.1(14) . . ? N1 C5 C6 116.8(13) . . ? C4 C5 C6 123.1(15) . . ? N2 C6 C5 124.9(12) . . ? N2 C6 H6A 117.5 . . ? C5 C6 H6A 117.5 . . ? N3 C7 C14 127.6(11) . . ? N3 C7 C8 116.1(11) . . ? C14 C7 C8 116.2(10) . . ? C13 C8 C9 119.2(10) . . ? C13 C8 C7 118.1(13) . . ? C9 C8 C7 122.6(12) . . ? C10 C9 C8 120.6(12) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C11 C10 C9 119.5(13) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C12 122.6(14) . . ? C10 C11 H11A 118.7 . . ? C12 C11 H11A 118.7 . . ? C11 C12 C13 119.2(12) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C8 C13 C12 118.7(11) . . ? C8 C13 H13A 120.7 . . ? C12 C13 H13A 120.7 . . ? N4 C14 C7 125.3(11) . . ? N4 C14 C15 116.4(12) . . ? C7 C14 C15 117.6(11) . . ? C20 C15 C16 119.5(11) . . ? C20 C15 C14 119.4(12) . . ? C16 C15 C14 121.1(14) . . ? C17 C16 C15 116.8(12) . . ? C17 C16 H16A 121.6 . . ? C15 C16 H16A 121.6 . . ? C18 C17 C16 123.4(16) . . ? C18 C17 H17A 118.3 . . ? C16 C17 H17A 118.3 . . ? C17 C18 C19 119.9(19) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C18 C19 C20 124.9(16) . . ? C18 C19 H19A 117.5 . . ? C20 C19 H19A 117.5 . . ? C19 C20 C15 115.4(12) . . ? C19 C20 H20A 122.3 . . ? C15 C20 H20A 122.3 . . ? N5 C21 C22 120.3(13) . . ? N5 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? N6 C22 C23 124.9(13) . . ? N6 C22 C21 121.1(14) . . ? C23 C22 C21 114.0(18) . . ? C24 C23 C22 117.4(15) . . ? C24 C23 H23A 121.3 . . ? C22 C23 H23A 121.3 . . ? C23 C24 C25 117.2(17) . . ? C23 C24 H24A 121.4 . . ? C25 C24 H24A 121.4 . . ? C24 C25 C26 124.8(16) . . ? C24 C25 H25A 117.6 . . ? C26 C25 H25A 117.6 . . ? N6 C26 C25 119.2(14) . . ? N6 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? O2 Cl1 O2 132.9(12) . 5 ? O2 Cl1 O4 45.3(7) . 5 ? O2 Cl1 O4 115.1(8) 5 5 ? O2 Cl1 O4 115.1(8) . . ? O2 Cl1 O4 45.3(7) 5 . ? O4 Cl1 O4 139.2(14) 5 . ? O2 Cl1 O3 110.3(7) . . ? O2 Cl1 O3 63.8(8) 5 . ? O4 Cl1 O3 65.8(8) 5 . ? O4 Cl1 O3 109.0(8) . . ? O2 Cl1 O3 63.8(8) . 5 ? O2 Cl1 O3 110.3(7) 5 5 ? O4 Cl1 O3 109.0(8) 5 5 ? O4 Cl1 O3 65.8(8) . 5 ? O3 Cl1 O3 166.2(13) . 5 ? O2 Cl1 O1 113.5(6) . . ? O2 Cl1 O1 113.5(6) 5 . ? O4 Cl1 O1 110.4(7) 5 . ? O4 Cl1 O1 110.4(7) . . ? O3 Cl1 O1 96.9(6) . . ? O3 Cl1 O1 96.9(6) 5 . ? O4 O2 Cl1 67.9(7) 5 . ? O4 O2 O3 127.9(11) 5 5 ? Cl1 O2 O3 60.0(6) . 5 ? Cl1 O3 O2 56.2(5) . 5 ? Cl1 O3 O4 55.6(5) . 5 ? O2 O3 O4 101.2(10) 5 5 ? O2 O4 Cl1 66.8(7) 5 . ? O2 O4 O3 124.2(12) 5 5 ? Cl1 O4 O3 58.6(6) . 5 ? O7 Cl2 O6 110.9(8) . . ? O7 Cl2 O9 110.2(8) . . ? O6 Cl2 O9 109.4(7) . . ? O7 Cl2 O8 109.3(7) . . ? O6 Cl2 O8 109.8(8) . . ? O9 Cl2 O8 107.2(7) . . ? O7 Cl2 O6 49.6(14) . 4_556 ? O6 Cl2 O6 63.6(16) . 4_556 ? O9 Cl2 O6 140.1(13) . 4_556 ? O8 Cl2 O6 112.0(13) . 4_556 ? O7 Cl2 O7 99.7(11) . 4_556 ? O6 Cl2 O7 45.7(12) . 4_556 ? O9 Cl2 O7 72.8(12) . 4_556 ? O8 Cl2 O7 148.4(12) . 4_556 ? O6 Cl2 O7 77.6(9) 4_556 4_556 ? O7 Cl2 Cl2 62.4(10) . 4_556 ? O6 Cl2 Cl2 56.4(11) . 4_556 ? O9 Cl2 Cl2 100.3(12) . 4_556 ? O8 Cl2 Cl2 152.3(12) . 4_556 ? O6 Cl2 Cl2 41.4(5) 4_556 4_556 ? O7 Cl2 Cl2 40.5(5) 4_556 4_556 ? O7 O6 Cl2 87.1(15) 4_556 . ? O7 O6 O6 97.0(17) 4_556 4_556 ? Cl2 O6 O6 68.7(12) . 4_556 ? O7 O6 Cl2 51.1(11) 4_556 4_556 ? Cl2 O6 Cl2 82.2(11) . 4_556 ? O6 O6 Cl2 47.7(10) 4_556 4_556 ? O6 O7 Cl2 79.3(19) 4_556 . ? O6 O7 Cl2 47.2(9) 4_556 4_556 ? Cl2 O7 Cl2 77.1(10) . 4_556 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.660 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.067 data_compound_1-P _database_code_depnum_ccdc_archive 'CCDC 603049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 Ag2 N18 O9' _chemical_formula_weight 1210.75 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' 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 P3(2)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 14.1473(5) _cell_length_b 14.1473(5) _cell_length_c 23.3160(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4041.4(4) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4604 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 20.07 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1842 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 20487 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4746 _reflns_number_gt 2649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(5) _refine_ls_number_reflns 4746 _refine_ls_number_parameters 328 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.1005 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1484 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.044 _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 0.17091(7) 0.27711(5) 0.84183(3) 0.0985(3) Uani 1 1 d . . . N1 N 0.3915(6) 0.6259(7) 0.8836(4) 0.107(3) Uani 1 1 d . . . H1B H 0.4450 0.6827 0.8990 0.128 Uiso 1 1 calc R . . N2 N 0.2822(5) 0.4574(5) 0.8627(3) 0.0789(17) Uani 1 1 d . . . N3 N 0.1024(4) 0.3749(4) 0.7858(2) 0.0585(13) Uani 1 1 d . . . N4 N 0.0085(5) 0.3473(5) 0.7539(2) 0.0618(15) Uani 1 1 d . . . N5 N 0.0419(5) 0.1334(5) 0.7183(2) 0.0631(14) Uani 1 1 d . . . N6 N -0.0432(5) 0.0771(5) 0.7574(3) 0.0682(16) Uani 1 1 d . . . N7 N -0.2026(5) -0.0636(5) 0.8414(3) 0.0759(16) Uani 1 1 d . . . N8 N -0.2411(7) -0.2278(6) 0.8605(3) 0.098(2) Uani 1 1 d . . . H8B H -0.2739 -0.2912 0.8763 0.118 Uiso 1 1 calc R . . C1 C 0.3673(7) 0.5232(9) 0.8937(4) 0.098(3) Uani 1 1 d . . . H1A H 0.4047 0.5020 0.9185 0.118 Uiso 1 1 calc R . . C2 C 0.3210(8) 0.6274(7) 0.8464(4) 0.091(3) Uani 1 1 d . . . H2A H 0.3203 0.6886 0.8324 0.109 Uiso 1 1 calc R . . C3 C 0.2503(6) 0.5216(6) 0.8331(3) 0.0633(18) Uani 1 1 d . . . C4 C 0.1548(7) 0.4747(7) 0.7977(3) 0.0664(18) Uani 1 1 d . . . H4A H 0.1306 0.5200 0.7829 0.080 Uiso 1 1 calc R . . C5 C -0.0167(5) 0.2717(6) 0.7171(3) 0.0563(16) Uani 1 1 d . . . C6 C -0.1134(5) 0.2406(5) 0.6808(3) 0.0589(16) Uani 1 1 d . . . C7 C -0.1575(7) 0.1494(7) 0.6489(4) 0.087(3) Uani 1 1 d . . . H7A H -0.1266 0.1048 0.6496 0.105 Uiso 1 1 calc R . . C8 C -0.2506(8) 0.1200(8) 0.6140(4) 0.104(3) Uani 1 1 d . . . H8A H -0.2821 0.0549 0.5935 0.125 Uiso 1 1 calc R . . C9 C -0.2938(8) 0.1872(11) 0.6106(4) 0.106(3) Uani 1 1 d . . . H9A H -0.3529 0.1703 0.5867 0.128 Uiso 1 1 calc R . . C10 C -0.2481(8) 0.2797(8) 0.6430(4) 0.099(3) Uani 1 1 d . . . H10A H -0.2786 0.3247 0.6420 0.118 Uiso 1 1 calc R . . C11 C -0.1581(7) 0.3087(7) 0.6773(3) 0.086(2) Uani 1 1 d . . . H11A H -0.1273 0.3736 0.6979 0.103 Uiso 1 1 calc R . . C12 C 0.1727(7) 0.3899(7) 0.6437(3) 0.081(2) Uani 1 1 d . . . H12A H 0.1313 0.4192 0.6578 0.097 Uiso 1 1 calc R . . C13 C 0.2563(9) 0.4517(8) 0.6064(4) 0.102(3) Uani 1 1 d . . . H13A H 0.2747 0.5232 0.5981 0.122 Uiso 1 1 calc R . . C14 C 0.3128(8) 0.4060(10) 0.5813(4) 0.109(3) Uani 1 1 d . . . H14A H 0.3639 0.4428 0.5526 0.130 Uiso 1 1 calc R . . C15 C 0.2911(7) 0.3029(10) 0.6002(4) 0.100(3) Uani 1 1 d . . . H15A H 0.3328 0.2732 0.5870 0.120 Uiso 1 1 calc R . . C16 C 0.2073(6) 0.2463(7) 0.6384(3) 0.080(2) Uani 1 1 d . . . H16A H 0.1904 0.1765 0.6496 0.096 Uiso 1 1 calc R . . C17 C 0.1478(6) 0.2903(6) 0.6606(3) 0.0590(17) Uani 1 1 d . . . C18 C 0.0564(5) 0.2261(6) 0.7008(3) 0.0544(16) Uani 1 1 d . . . C19 C -0.0599(6) -0.0198(5) 0.7673(3) 0.0667(18) Uani 1 1 d . . . H19A H -0.0181 -0.0429 0.7473 0.080 Uiso 1 1 calc R . . C20 C -0.1402(6) -0.0949(6) 0.8079(3) 0.071(2) Uani 1 1 d . . . C21 C -0.1651(7) -0.1964(6) 0.8205(4) 0.080(2) Uani 1 1 d . . . H21A H -0.1356 -0.2364 0.8047 0.096 Uiso 1 1 calc R . . C22 C -0.2596(7) -0.1438(7) 0.8728(4) 0.089(2) Uani 1 1 d . . . H22A H -0.3078 -0.1462 0.9006 0.107 Uiso 1 1 calc R . . C23 C 0.508(3) 0.868(2) 0.9198(13) 0.155(10) Uiso 0.50 1 d PDU A 1 O4 O 0.4956(16) 0.9636(16) 0.8854(8) 0.169(6) Uiso 0.50 1 d PDU A 1 C23' C 0.5486(19) 0.9631(17) 0.9287(10) 0.130(7) Uiso 0.50 1 d PDU B 2 O4' O 0.5182(11) 0.8349(10) 0.9394(5) 0.096(4) Uiso 0.50 1 d PDU B 2 N9 N 0.5370(11) 0.7373(12) 1.0577(5) 0.195(5) Uiso 1 1 d DU . . O1 O 0.6241(15) 0.740(2) 1.0478(9) 0.198(7) Uiso 0.50 1 d PDU C 1 O2 O 0.4816(12) 0.7747(12) 1.0372(7) 0.120(4) Uiso 0.50 1 d PDU C 1 O3 O 0.5375(13) 0.7376(14) 1.1097(5) 0.131(5) Uiso 0.50 1 d PDU C 1 O3' O 0.5640(18) 0.6888(18) 1.0911(8) 0.187(6) Uiso 0.50 1 d PDU C 2 O2' O 0.4707(12) 0.7618(14) 1.0706(7) 0.137(6) Uiso 0.50 1 d PD C 2 O1' O 0.5447(17) 0.7214(17) 1.0050(7) 0.182(7) Uiso 0.50 1 d PD C 2 O1W O 0.5955(16) 0.6397(15) 0.9498(8) 0.166(6) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.1193(6) 0.0649(4) 0.1191(5) 0.0051(4) -0.0131(5) 0.0519(4) N1 0.072(5) 0.085(6) 0.114(6) -0.024(5) 0.016(5) 0.002(4) N2 0.071(4) 0.069(4) 0.087(4) -0.015(3) -0.001(4) 0.028(4) N3 0.069(4) 0.043(3) 0.064(3) -0.010(3) -0.009(3) 0.029(3) N4 0.065(4) 0.058(4) 0.068(4) -0.004(3) -0.011(3) 0.036(3) N5 0.062(4) 0.054(4) 0.071(4) -0.007(3) 0.001(3) 0.028(3) N6 0.067(4) 0.056(4) 0.084(4) -0.004(3) -0.008(3) 0.031(3) N7 0.069(4) 0.056(4) 0.088(4) 0.010(4) 0.001(3) 0.020(4) N8 0.107(6) 0.054(4) 0.117(6) 0.012(4) -0.005(5) 0.026(4) C1 0.070(6) 0.086(7) 0.124(7) -0.020(6) -0.022(5) 0.028(5) C2 0.076(6) 0.075(6) 0.094(6) -0.024(5) 0.008(5) 0.017(5) C3 0.058(4) 0.053(4) 0.073(5) -0.001(4) 0.009(4) 0.024(4) C4 0.084(5) 0.073(5) 0.061(4) -0.001(4) 0.003(4) 0.053(5) C5 0.057(4) 0.048(4) 0.067(4) 0.005(4) 0.005(3) 0.029(3) C6 0.051(4) 0.062(4) 0.065(4) 0.000(3) -0.001(3) 0.029(4) C7 0.071(6) 0.088(6) 0.121(7) -0.034(5) -0.020(5) 0.054(5) C8 0.088(6) 0.133(8) 0.118(7) -0.056(6) -0.042(6) 0.075(7) C9 0.080(6) 0.174(10) 0.080(6) -0.006(6) -0.018(5) 0.074(7) C10 0.115(7) 0.116(7) 0.101(7) -0.012(6) -0.030(6) 0.085(6) C11 0.090(6) 0.098(6) 0.094(6) -0.002(5) -0.004(6) 0.064(6) C12 0.085(6) 0.081(6) 0.079(5) 0.004(4) 0.015(4) 0.042(5) C13 0.121(8) 0.105(6) 0.091(6) 0.030(5) 0.036(6) 0.065(6) C14 0.082(6) 0.147(10) 0.093(7) 0.029(6) 0.019(5) 0.054(7) C15 0.065(6) 0.142(9) 0.093(6) -0.014(6) 0.005(5) 0.051(6) C16 0.062(5) 0.094(6) 0.090(5) -0.011(5) -0.008(5) 0.044(5) C17 0.052(4) 0.072(5) 0.059(4) -0.006(4) -0.002(3) 0.036(4) C18 0.053(4) 0.052(4) 0.062(4) -0.002(3) -0.006(3) 0.029(4) C19 0.074(5) 0.047(4) 0.085(5) -0.005(4) -0.003(4) 0.034(4) C20 0.079(5) 0.055(5) 0.082(5) -0.010(4) -0.001(4) 0.036(4) C21 0.073(6) 0.047(5) 0.110(6) 0.005(4) 0.016(5) 0.023(4) C22 0.082(6) 0.065(5) 0.100(6) -0.007(5) 0.007(5) 0.022(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N7 2.246(6) 6_556 ? Ag1 N2 2.282(6) . ? Ag1 N3 2.429(5) . ? Ag1 N6 2.579(6) 6_556 ? N1 C2 1.331(11) . ? N1 C1 1.335(12) . ? N2 C1 1.310(10) . ? N2 C3 1.385(9) . ? N3 C4 1.254(9) . ? N3 N4 1.398(7) . ? N4 C5 1.275(8) . ? N5 C18 1.289(8) . ? N5 N6 1.399(8) . ? N6 C19 1.290(8) . ? N6 Ag1 2.579(6) 6_556 ? N7 C22 1.248(10) . ? N7 C20 1.407(9) . ? N7 Ag1 2.246(6) 6_556 ? N8 C21 1.322(10) . ? N8 C22 1.369(11) . ? C2 C3 1.357(11) . ? C3 C4 1.432(10) . ? C5 C6 1.475(9) . ? C5 C18 1.515(10) . ? C6 C7 1.343(10) . ? C6 C11 1.395(10) . ? C7 C8 1.422(11) . ? C8 C9 1.367(13) . ? C9 C10 1.361(12) . ? C10 C11 1.381(12) . ? C12 C17 1.331(10) . ? C12 C13 1.373(11) . ? C13 C14 1.383(13) . ? C14 C15 1.404(13) . ? C15 C16 1.377(12) . ? C16 C17 1.373(10) . ? C17 C18 1.483(10) . ? C19 C20 1.452(10) . ? C20 C21 1.329(10) . ? C23 O4 1.66(2) . ? C23' O4' 1.66(2) . ? N9 O2' 1.190(10) . ? N9 O3 1.211(9) . ? N9 O3' 1.220(10) . ? N9 O1 1.233(10) . ? N9 O2 1.239(9) . ? N9 O1' 1.263(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 N7 Ag1 N2 133.1(2) 6_556 . ? N7 Ag1 N3 135.5(2) 6_556 . ? N2 Ag1 N3 74.2(2) . . ? N7 Ag1 N6 73.5(2) 6_556 6_556 ? N2 Ag1 N6 128.8(2) . 6_556 ? N3 Ag1 N6 120.68(18) . 6_556 ? C2 N1 C1 110.2(8) . . ? C1 N2 C3 107.1(7) . . ? C1 N2 Ag1 142.0(7) . . ? C3 N2 Ag1 110.9(5) . . ? C4 N3 N4 112.1(6) . . ? C4 N3 Ag1 110.1(5) . . ? N4 N3 Ag1 136.2(4) . . ? C5 N4 N3 114.9(5) . . ? C18 N5 N6 116.1(5) . . ? C19 N6 N5 111.7(6) . . ? C19 N6 Ag1 106.8(5) . 6_556 ? N5 N6 Ag1 141.2(4) . 6_556 ? C22 N7 C20 105.1(7) . . ? C22 N7 Ag1 140.0(7) . 6_556 ? C20 N7 Ag1 114.9(5) . 6_556 ? C21 N8 C22 109.4(7) . . ? N2 C1 N1 108.8(9) . . ? N1 C2 C3 106.0(9) . . ? C2 C3 N2 107.9(7) . . ? C2 C3 C4 130.3(8) . . ? N2 C3 C4 121.7(7) . . ? N3 C4 C3 122.5(7) . . ? N4 C5 C6 117.6(6) . . ? N4 C5 C18 124.2(6) . . ? C6 C5 C18 117.2(6) . . ? C7 C6 C11 118.5(7) . . ? C7 C6 C5 121.3(6) . . ? C11 C6 C5 120.1(7) . . ? C6 C7 C8 121.0(7) . . ? C9 C8 C7 120.1(8) . . ? C10 C9 C8 118.3(8) . . ? C9 C10 C11 122.1(8) . . ? C10 C11 C6 119.9(8) . . ? C17 C12 C13 123.4(8) . . ? C12 C13 C14 119.0(9) . . ? C13 C14 C15 118.5(9) . . ? C16 C15 C14 118.9(9) . . ? C17 C16 C15 121.8(9) . . ? C12 C17 C16 118.0(8) . . ? C12 C17 C18 121.6(6) . . ? C16 C17 C18 120.4(7) . . ? N5 C18 C17 117.9(6) . . ? N5 C18 C5 124.0(6) . . ? C17 C18 C5 118.0(6) . . ? N6 C19 C20 123.7(6) . . ? C21 C20 N7 110.4(7) . . ? C21 C20 C19 128.5(7) . . ? N7 C20 C19 121.1(6) . . ? N8 C21 C20 104.5(7) . . ? N7 C22 N8 110.5(8) . . ? O2' N9 O3 75.5(11) . . ? O2' N9 O3' 121.1(12) . . ? O3 N9 O3' 50.2(10) . . ? O2' N9 O1 163(2) . . ? O3 N9 O1 100.5(14) . . ? O3' N9 O1 63.2(13) . . ? O2' N9 O2 38.3(9) . . ? O3 N9 O2 112.9(13) . . ? O3' N9 O2 158.4(15) . . ? O1 N9 O2 138.3(18) . . ? O2' N9 O1' 116.7(11) . . ? O3 N9 O1' 166.4(13) . . ? O3' N9 O1' 116.2(11) . . ? O1 N9 O1' 69.6(13) . . ? O2 N9 O1' 80.2(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.541 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.085 # Attachment 'compound 1-M.txt' data_compound_1-M _database_code_depnum_ccdc_archive 'CCDC 603050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 Ag2 N18 O9' _chemical_formula_weight 1210.75 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' 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 P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 14.165(1) _cell_length_b 14.165(1) _cell_length_c 23.145(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4021.8(7) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6238 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 22.55 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1842 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 20254 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4743 _reflns_number_gt 3245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(5) _refine_ls_number_reflns 4743 _refine_ls_number_parameters 329 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1673 _refine_ls_wR_factor_gt 0.1567 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.088 _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 0.72145(5) 0.89291(5) 0.49154(3) 0.1018(3) Uani 1 1 d . . . N1 N 0.9831(7) 1.2254(5) 0.5293(4) 0.103(2) Uani 1 1 d . . . H1A H 1.0132 1.2884 0.5455 0.123 Uiso 1 1 calc R . . N2 N 0.8579(5) 1.0611(5) 0.5089(3) 0.0792(15) Uani 1 1 d . . . N3 N 0.8773(4) 0.9225(4) 0.4239(2) 0.0677(14) Uani 1 1 d . . . N4 N 0.9066(4) 0.8672(4) 0.3845(2) 0.0642(12) Uani 1 1 d . . . N5 N 0.6601(4) 0.6517(4) 0.4200(2) 0.0670(13) Uani 1 1 d . . . N6 N 0.7262(4) 0.6232(4) 0.4518(2) 0.0641(12) Uani 1 1 d . . . N7 N 0.8238(5) 0.5415(5) 0.5290(3) 0.0825(16) Uani 1 1 d . . . N8 N 0.7638(8) 0.3716(6) 0.5497(4) 0.109(3) Uani 1 1 d . . . H8A H 0.7606 0.3144 0.5645 0.130 Uiso 1 1 calc R . . C1 C 0.8829(8) 1.1430(6) 0.5408(4) 0.093(2) Uani 1 1 d . . . H1B H 0.8372 1.1455 0.5689 0.111 Uiso 1 1 calc R . . C2 C 1.0292(7) 1.1946(6) 0.4886(4) 0.083(2) Uani 1 1 d . . . H2A H 1.0988 1.2350 0.4730 0.100 Uiso 1 1 calc R . . C3 C 0.9522(5) 1.0918(5) 0.4753(3) 0.0731(17) Uani 1 1 d . . . C4 C 0.9583(5) 1.0194(5) 0.4333(3) 0.0690(16) Uani 1 1 d . . . H4B H 1.0224 1.0433 0.4124 0.083 Uiso 1 1 calc R . . C5 C 0.8296(5) 0.7754(5) 0.3673(3) 0.0555(13) Uani 1 1 d . . . C6 C 0.8575(5) 0.7111(5) 0.3268(3) 0.0623(15) Uani 1 1 d . . . C7 C 0.7812(7) 0.6096(6) 0.3094(4) 0.086(2) Uani 1 1 d . . . H7B H 0.7106 0.5789 0.3237 0.103 Uiso 1 1 calc R . . C8 C 0.8064(8) 0.5507(7) 0.2706(4) 0.105(3) Uani 1 1 d . . . H8B H 0.7533 0.4802 0.2606 0.126 Uiso 1 1 calc R . . C9 C 0.9061(10) 0.5942(10) 0.2476(4) 0.113(3) Uani 1 1 d . . . H9A H 0.9211 0.5562 0.2197 0.136 Uiso 1 1 calc R . . C10 C 0.9872(8) 0.6965(9) 0.2657(4) 0.101(3) Uani 1 1 d . . . H10A H 1.0580 0.7255 0.2519 0.121 Uiso 1 1 calc R . . C11 C 0.9615(5) 0.7555(7) 0.3046(3) 0.0781(19) Uani 1 1 d . . . H11A H 1.0149 0.8252 0.3156 0.094 Uiso 1 1 calc R . . C12 C 0.5325(6) 0.6912(7) 0.3432(4) 0.095(2) Uani 1 1 d . . . H12A H 0.4984 0.6260 0.3637 0.114 Uiso 1 1 calc R . . C13 C 0.4722(7) 0.7205(9) 0.3091(4) 0.106(3) Uani 1 1 d . . . H13A H 0.3969 0.6753 0.3082 0.127 Uiso 1 1 calc R . . C14 C 0.5177(8) 0.8131(10) 0.2766(4) 0.107(3) Uani 1 1 d . . . H14A H 0.4758 0.8303 0.2526 0.128 Uiso 1 1 calc R . . C15 C 0.6284(7) 0.8794(8) 0.2809(4) 0.105(3) Uani 1 1 d . . . H15A H 0.6622 0.9452 0.2609 0.126 Uiso 1 1 calc R . . C16 C 0.6908(6) 0.8509(7) 0.3143(3) 0.085(2) Uani 1 1 d . . . H16A H 0.7662 0.8956 0.3143 0.102 Uiso 1 1 calc R . . C17 C 0.6451(5) 0.7592(5) 0.3470(3) 0.0623(14) Uani 1 1 d . . . C18 C 0.7104(5) 0.7275(5) 0.3826(3) 0.0583(14) Uani 1 1 d . . . C19 C 0.6782(5) 0.5224(6) 0.4636(3) 0.0704(17) Uani 1 1 d . . . H19A H 0.6087 0.4765 0.4490 0.085 Uiso 1 1 calc R . . C20 C 0.7294(5) 0.4782(6) 0.4992(3) 0.0683(16) Uani 1 1 d . . . C21 C 0.6929(8) 0.3719(6) 0.5126(4) 0.094(2) Uani 1 1 d . . . H21A H 0.6304 0.3115 0.4985 0.113 Uiso 1 1 calc R . . C22 C 0.8424(8) 0.4758(8) 0.5604(5) 0.108(3) Uani 1 1 d . . . H22A H 0.9002 0.4972 0.5861 0.130 Uiso 1 1 calc R . . C23 C 0.544(2) 0.956(2) 0.0714(12) 0.178(9) Uiso 0.65 1 d P A 1 O4 O 0.5134(10) 0.8401(10) 0.0654(5) 0.127(3) Uiso 0.65 1 d P A 1 C23' C 0.474(3) 0.989(3) 0.1169(14) 0.128(10) Uiso 0.35 1 d P B 2 O4' O 0.514(2) 0.954(2) 0.1153(12) 0.152(8) Uiso 0.35 1 d P B 2 N9 N 0.5342(11) 0.7393(11) -0.0643(5) 0.165(4) Uiso 1 1 d DU . . O1 O 0.4824(12) 0.7717(12) -0.0386(7) 0.127(4) Uiso 0.560(12) 1 d PDU C 1 O2 O 0.6123(17) 0.7305(19) -0.0481(9) 0.192(5) Uiso 0.560(12) 1 d PDU C 1 O3 O 0.5408(16) 0.7396(17) -0.1139(7) 0.167(5) Uiso 0.560(12) 1 d PDU C 1 O1' O 0.546(2) 0.7281(19) -0.0083(8) 0.168(6) Uiso 0.440(12) 1 d PDU C 2 O2' O 0.560(2) 0.688(2) -0.0932(10) 0.173(6) Uiso 0.440(12) 1 d PDU C 2 O3' O 0.4754(15) 0.7678(17) -0.0724(9) 0.142(5) Uiso 0.440(12) 1 d PDU C 2 O1W O 0.623(2) 0.607(2) -0.0536(10) 0.199(8) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0630(3) 0.0787(4) 0.1329(5) 0.0196(4) 0.0041(3) 0.0124(3) N1 0.102(5) 0.052(3) 0.143(6) -0.015(4) -0.017(5) 0.030(4) N2 0.087(4) 0.054(3) 0.098(4) 0.001(3) 0.004(3) 0.037(3) N3 0.054(3) 0.050(3) 0.097(4) 0.004(3) 0.000(3) 0.024(3) N4 0.052(3) 0.056(3) 0.085(3) 0.011(3) 0.010(3) 0.027(3) N5 0.052(3) 0.057(3) 0.080(3) 0.003(3) -0.005(3) 0.019(3) N6 0.059(3) 0.048(3) 0.078(3) 0.009(2) 0.000(3) 0.022(2) N7 0.079(4) 0.065(3) 0.103(4) 0.018(3) 0.010(3) 0.035(3) N8 0.142(7) 0.069(4) 0.129(6) 0.019(4) 0.032(6) 0.063(5) C1 0.099(6) 0.061(4) 0.120(6) 0.004(4) 0.002(5) 0.041(4) C2 0.074(5) 0.053(4) 0.113(6) -0.004(4) 0.004(4) 0.025(4) C3 0.061(4) 0.051(3) 0.093(5) 0.009(3) 0.009(4) 0.018(3) C4 0.055(3) 0.049(3) 0.087(4) 0.005(3) 0.006(3) 0.013(3) C5 0.041(3) 0.047(3) 0.074(4) 0.006(3) 0.003(3) 0.019(3) C6 0.054(3) 0.065(4) 0.073(4) 0.007(3) 0.002(3) 0.034(3) C7 0.077(5) 0.076(5) 0.103(5) -0.008(4) 0.004(4) 0.036(4) C8 0.102(6) 0.096(5) 0.120(7) -0.036(5) 0.003(6) 0.053(5) C9 0.135(9) 0.130(9) 0.117(7) -0.024(6) 0.006(6) 0.099(8) C10 0.100(6) 0.136(8) 0.105(6) 0.016(6) 0.025(5) 0.088(7) C11 0.057(4) 0.084(5) 0.101(5) 0.018(4) 0.010(3) 0.041(4) C12 0.052(4) 0.098(6) 0.118(6) 0.013(5) -0.006(4) 0.025(4) C13 0.064(4) 0.127(8) 0.123(7) -0.004(6) -0.026(5) 0.045(5) C14 0.102(7) 0.156(9) 0.099(6) 0.013(6) -0.007(5) 0.091(7) C15 0.071(5) 0.132(7) 0.119(6) 0.051(6) 0.012(5) 0.056(5) C16 0.054(3) 0.091(5) 0.111(5) 0.026(4) 0.014(4) 0.036(4) C17 0.055(3) 0.065(4) 0.072(3) -0.003(3) 0.001(3) 0.033(3) C18 0.050(3) 0.044(3) 0.074(4) -0.002(3) -0.002(3) 0.018(3) C19 0.054(3) 0.057(4) 0.080(4) 0.000(3) 0.007(3) 0.012(3) C20 0.068(4) 0.061(4) 0.079(4) 0.003(3) 0.011(4) 0.034(3) C21 0.104(6) 0.061(4) 0.114(6) 0.026(4) 0.029(5) 0.040(4) C22 0.106(6) 0.104(7) 0.139(7) 0.021(6) 0.006(6) 0.071(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.229(6) . ? Ag1 N7 2.277(6) 4_556 ? Ag1 N6 2.438(5) 4_556 ? Ag1 N3 2.564(5) . ? N1 C2 1.337(10) . ? N1 C1 1.338(12) . ? N2 C1 1.267(10) . ? N2 C3 1.413(9) . ? N3 C4 1.294(8) . ? N3 N4 1.393(8) . ? N4 C5 1.274(8) . ? N5 C18 1.281(8) . ? N5 N6 1.400(8) . ? N6 C19 1.267(8) . ? N6 Ag1 2.438(5) 4_556 ? N7 C22 1.309(10) . ? N7 C20 1.367(9) . ? N7 Ag1 2.277(6) 4_556 ? N8 C21 1.323(12) . ? N8 C22 1.356(13) . ? C2 C3 1.349(10) . ? C3 C4 1.445(10) . ? C5 C6 1.491(9) . ? C5 C18 1.514(9) . ? C6 C7 1.358(10) . ? C6 C11 1.380(9) . ? C7 C8 1.388(11) . ? C8 C9 1.338(14) . ? C9 C10 1.389(14) . ? C10 C11 1.395(12) . ? C12 C13 1.370(13) . ? C12 C17 1.394(10) . ? C13 C14 1.363(13) . ? C14 C15 1.371(13) . ? C15 C16 1.378(11) . ? C16 C17 1.356(10) . ? C17 C18 1.467(9) . ? C19 C20 1.432(10) . ? C20 C21 1.360(11) . ? C23 O4 1.48(3) . ? C23' O4' 0.91(4) . ? N9 O3' 1.108(14) . ? N9 O3 1.151(13) . ? N9 O2' 1.166(15) . ? N9 O1 1.200(13) . ? N9 O2 1.232(14) . ? N9 O1' 1.326(15) . ? 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 N7 133.1(2) . 4_556 ? N2 Ag1 N6 135.10(19) . 4_556 ? N7 Ag1 N6 73.8(2) 4_556 4_556 ? N2 Ag1 N3 73.7(2) . . ? N7 Ag1 N3 129.1(2) 4_556 . ? N6 Ag1 N3 120.93(17) 4_556 . ? C2 N1 C1 109.5(7) . . ? C1 N2 C3 104.5(7) . . ? C1 N2 Ag1 141.2(6) . . ? C3 N2 Ag1 114.2(4) . . ? C4 N3 N4 110.6(5) . . ? C4 N3 Ag1 107.8(4) . . ? N4 N3 Ag1 141.4(4) . . ? C5 N4 N3 115.8(5) . . ? C18 N5 N6 115.1(5) . . ? C19 N6 N5 112.3(5) . . ? C19 N6 Ag1 110.4(4) . 4_556 ? N5 N6 Ag1 135.6(4) . 4_556 ? C22 N7 C20 107.0(7) . . ? C22 N7 Ag1 141.8(7) . 4_556 ? C20 N7 Ag1 111.2(4) . 4_556 ? C21 N8 C22 109.1(7) . . ? N2 C1 N1 111.8(8) . . ? N1 C2 C3 104.5(7) . . ? C2 C3 N2 109.6(7) . . ? C2 C3 C4 128.1(7) . . ? N2 C3 C4 122.3(6) . . ? N3 C4 C3 122.0(6) . . ? N4 C5 C6 117.9(5) . . ? N4 C5 C18 125.3(5) . . ? C6 C5 C18 116.8(5) . . ? C7 C6 C11 118.4(7) . . ? C7 C6 C5 121.3(6) . . ? C11 C6 C5 120.3(6) . . ? C6 C7 C8 121.4(8) . . ? C9 C8 C7 120.7(9) . . ? C8 C9 C10 119.5(8) . . ? C9 C10 C11 119.5(8) . . ? C6 C11 C10 120.4(8) . . ? C13 C12 C17 119.9(8) . . ? C14 C13 C12 122.9(8) . . ? C13 C14 C15 116.6(8) . . ? C14 C15 C16 121.4(8) . . ? C17 C16 C15 121.7(7) . . ? C16 C17 C12 117.4(6) . . ? C16 C17 C18 122.4(6) . . ? C12 C17 C18 120.2(6) . . ? N5 C18 C17 117.7(5) . . ? N5 C18 C5 124.2(5) . . ? C17 C18 C5 117.6(5) . . ? N6 C19 C20 120.8(6) . . ? C21 C20 N7 108.5(7) . . ? C21 C20 C19 128.3(8) . . ? N7 C20 C19 123.1(6) . . ? N8 C21 C20 106.4(8) . . ? N7 C22 N8 108.9(9) . . ? O3' N9 O3 84.6(16) . . ? O3' N9 O2' 130.7(17) . . ? O3 N9 O2' 51.7(13) . . ? O3' N9 O1 39.6(10) . . ? O3 N9 O1 123.9(17) . . ? O2' N9 O1 164(2) . . ? O3' N9 O2 165(2) . . ? O3 N9 O2 103.2(16) . . ? O2' N9 O2 62.6(14) . . ? O1 N9 O2 129.7(17) . . ? O3' N9 O1' 111.4(15) . . ? O3 N9 O1' 163.9(17) . . ? O2' N9 O1' 113.2(15) . . ? O1 N9 O1' 72.2(12) . . ? O2 N9 O1' 61.4(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.709 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.093 # Attachment 'compound 2-P.txt' data_compound_2-P _database_code_depnum_ccdc_archive 'CCDC 603051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 Ag2 Cl1.67 N12.33 O7.67' _chemical_formula_weight 1235.12 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(2)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 15.3556(18) _cell_length_b 15.3556(18) _cell_length_c 21.479(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4386.1(12) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4874 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 20.00 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1866 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 21961 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5161 _reflns_number_gt 3796 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 5161 _refine_ls_number_parameters 352 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1539 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.146 _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 0.35687(5) 0.47235(5) 0.03941(3) 0.0823(3) Uani 1 1 d . . . N1 N 0.2051(5) 0.3372(5) 0.0584(3) 0.0710(18) Uani 1 1 d . . . N2 N 0.2843(5) 0.3915(4) -0.0606(3) 0.0606(15) Uani 1 1 d . . . N3 N 0.3112(5) 0.3995(5) -0.1243(3) 0.0632(16) Uani 1 1 d . . . N4 N 0.5183(5) 0.5992(5) -0.0720(3) 0.0596(16) Uani 1 1 d . . . N5 N 0.5501(5) 0.5284(4) -0.0738(2) 0.0591(14) Uani 1 1 d . . . N6 N 0.6355(5) 0.4062(6) -0.0593(3) 0.0650(16) Uani 1 1 d . . . C1 C 0.1633(8) 0.3082(8) 0.1138(5) 0.091(3) Uani 1 1 d . . . H1A H 0.2006 0.3406 0.1491 0.109 Uiso 1 1 calc R . . C2 C 0.0663(9) 0.2313(11) 0.1205(6) 0.120(4) Uani 1 1 d . . . H2A H 0.0387 0.2132 0.1602 0.143 Uiso 1 1 calc R . . C3 C 0.0102(12) 0.1814(12) 0.0709(7) 0.162(7) Uani 1 1 d . . . H3B H -0.0561 0.1300 0.0753 0.195 Uiso 1 1 calc R . . C4 C 0.0547(9) 0.2094(10) 0.0138(6) 0.133(5) Uani 1 1 d . . . H4B H 0.0195 0.1755 -0.0217 0.160 Uiso 1 1 calc R . . C5 C 0.1512(6) 0.2874(7) 0.0091(4) 0.078(2) Uani 1 1 d . . . C6 C 0.1983(7) 0.3176(6) -0.0514(4) 0.072(2) Uani 1 1 d . . . H6B H 0.1624 0.2796 -0.0857 0.086 Uiso 1 1 calc R . . C7 C 0.3818(5) 0.4848(5) -0.1418(3) 0.0555(17) Uani 1 1 d . . . C8 C 0.4081(6) 0.5003(6) -0.2086(3) 0.0625(18) Uani 1 1 d . . . C9 C 0.4990(7) 0.5781(7) -0.2276(4) 0.074(2) Uani 1 1 d . . . H9A H 0.5446 0.6220 -0.1985 0.089 Uiso 1 1 calc R . . C10 C 0.5228(9) 0.5912(8) -0.2908(4) 0.091(3) Uani 1 1 d . . . H10A H 0.5842 0.6438 -0.3044 0.109 Uiso 1 1 calc R . . C11 C 0.4542(11) 0.5253(10) -0.3319(4) 0.102(4) Uani 1 1 d . . . H11A H 0.4700 0.5335 -0.3741 0.123 Uiso 1 1 calc R . . C12 C 0.3647(9) 0.4488(8) -0.3140(4) 0.095(3) Uani 1 1 d . . . H12A H 0.3196 0.4044 -0.3432 0.113 Uiso 1 1 calc R . . C13 C 0.3416(7) 0.4375(7) -0.2525(3) 0.082(2) Uani 1 1 d . . . H13A H 0.2789 0.3859 -0.2398 0.098 Uiso 1 1 calc R . . C14 C 0.4380(6) 0.5763(5) -0.1003(3) 0.0545(17) Uani 1 1 d . . . C15 C 0.4003(7) 0.6477(6) -0.0996(3) 0.065(2) Uani 1 1 d . . . C16 C 0.2996(7) 0.6183(7) -0.1108(3) 0.072(2) Uani 1 1 d . . . H16A H 0.2531 0.5514 -0.1194 0.086 Uiso 1 1 calc R . . C17 C 0.2702(8) 0.6883(9) -0.1090(4) 0.081(3) Uani 1 1 d . . . H17A H 0.2026 0.6680 -0.1148 0.097 Uiso 1 1 calc R . . C18 C 0.3345(12) 0.7841(11) -0.0992(4) 0.104(4) Uani 1 1 d . . . H18A H 0.3112 0.8296 -0.0997 0.125 Uiso 1 1 calc R . . C19 C 0.4377(10) 0.8205(7) -0.0878(4) 0.090(3) Uani 1 1 d . . . H19A H 0.4825 0.8882 -0.0803 0.108 Uiso 1 1 calc R . . C20 C 0.4671(8) 0.7515(6) -0.0884(3) 0.078(2) Uani 1 1 d . . . H20A H 0.5346 0.7728 -0.0813 0.093 Uiso 1 1 calc R . . C21 C 0.6460(6) 0.5673(6) -0.0749(3) 0.063(2) Uani 1 1 d . . . H21A H 0.6858 0.6368 -0.0778 0.076 Uiso 1 1 calc R . . C22 C 0.6944(6) 0.5085(7) -0.0718(3) 0.065(2) Uani 1 1 d . . . C23 C 0.7949(7) 0.5501(8) -0.0796(4) 0.088(3) Uani 1 1 d . . . H23A H 0.8342 0.6194 -0.0843 0.106 Uiso 1 1 calc R . . C24 C 0.8414(8) 0.4912(11) -0.0807(4) 0.094(3) Uani 1 1 d . . . H24A H 0.9094 0.5194 -0.0899 0.113 Uiso 1 1 calc R . . C25 C 0.7848(9) 0.3943(10) -0.0682(4) 0.092(3) Uani 1 1 d . . . H25A H 0.8137 0.3537 -0.0659 0.111 Uiso 1 1 calc R . . C26 C 0.6802(8) 0.3525(8) -0.0584(4) 0.078(3) Uani 1 1 d . . . H26A H 0.6415 0.2838 -0.0510 0.094 Uiso 1 1 calc R . . Cl1 Cl 0.7726(2) 0.0000 0.1667 0.0934(9) Uani 1 2 d S . . O11 O 0.7461(9) 0.0522(8) 0.1255(4) 0.155(4) Uani 1 1 d . . . O12 O 0.7927(7) -0.0673(8) 0.1336(4) 0.138(3) Uani 1 1 d . . . Cl2 Cl 0.0000 0.3493(3) -0.1667 0.0828(11) Uani 0.67 2 d SPDU . 1 O21 O 0.0000 0.4453(8) -0.1667 0.139(5) Uiso 0.67 2 d SPDU A 1 O22 O 0.0988(10) 0.3678(13) -0.1810(8) 0.101(3) Uiso 0.33 1 d PDU . 1 O23 O -0.0662(12) 0.3008(12) -0.2198(7) 0.105(3) Uiso 0.33 1 d PDU . 1 O24 O -0.0418(13) 0.2974(12) -0.1096(6) 0.101(3) Uiso 0.33 1 d PDU . 1 N7 N 0.0000 0.3493(3) -0.1667 0.0828(11) Uani 0.33 2 d SPDU . 2 O21' O -0.0883(14) 0.333(2) -0.1818(18) 0.086(4) Uiso 0.17 1 d PDU . 2 O22' O 0.032(2) 0.292(2) -0.1875(15) 0.090(3) Uiso 0.17 1 d PDU . 2 O23' O 0.0562(19) 0.425(2) -0.1312(16) 0.089(4) Uiso 0.17 1 d PDU . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0684(4) 0.0689(4) 0.0858(4) -0.0031(3) -0.0107(3) 0.0165(3) N1 0.070(4) 0.077(4) 0.059(4) 0.003(3) 0.005(3) 0.031(4) N2 0.071(4) 0.050(3) 0.056(4) 0.005(3) 0.003(3) 0.027(3) N3 0.076(5) 0.066(4) 0.045(3) -0.005(3) -0.006(3) 0.034(4) N4 0.083(5) 0.053(4) 0.043(3) 0.002(3) 0.001(3) 0.034(4) N5 0.062(4) 0.059(3) 0.045(3) 0.000(3) -0.005(3) 0.023(3) N6 0.071(4) 0.075(4) 0.048(3) -0.003(3) 0.000(3) 0.035(4) C1 0.091(7) 0.096(7) 0.078(6) 0.007(5) 0.019(5) 0.040(6) C2 0.092(8) 0.137(10) 0.097(8) 0.005(8) 0.032(7) 0.033(8) C3 0.106(10) 0.154(13) 0.120(10) 0.002(10) 0.026(8) -0.014(9) C4 0.087(8) 0.124(10) 0.112(9) 0.003(8) 0.019(7) -0.005(7) C5 0.054(5) 0.070(6) 0.089(6) 0.003(5) -0.004(5) 0.016(4) C6 0.069(5) 0.063(5) 0.066(5) -0.013(4) -0.008(4) 0.020(5) C7 0.062(4) 0.047(4) 0.056(4) 0.000(3) -0.005(3) 0.026(4) C8 0.086(5) 0.063(5) 0.046(4) -0.004(4) -0.002(4) 0.043(4) C9 0.101(7) 0.067(5) 0.065(5) 0.007(4) 0.015(5) 0.048(5) C10 0.139(9) 0.098(7) 0.060(6) 0.020(5) 0.025(6) 0.078(7) C11 0.184(12) 0.127(10) 0.045(5) -0.005(6) 0.001(6) 0.114(10) C12 0.128(9) 0.092(7) 0.056(5) -0.004(5) -0.002(5) 0.049(7) C13 0.102(7) 0.085(6) 0.056(5) -0.003(4) -0.001(4) 0.045(6) C14 0.065(5) 0.053(4) 0.043(4) 0.002(3) 0.007(3) 0.027(4) C15 0.097(6) 0.066(5) 0.039(4) 0.003(3) 0.003(4) 0.045(5) C16 0.088(6) 0.087(6) 0.051(4) 0.010(4) 0.005(4) 0.052(5) C17 0.111(7) 0.091(7) 0.058(5) 0.014(5) 0.021(5) 0.063(7) C18 0.192(13) 0.115(10) 0.060(5) 0.017(6) 0.017(6) 0.118(11) C19 0.149(10) 0.063(6) 0.083(6) 0.006(4) 0.011(6) 0.072(7) C20 0.110(7) 0.070(5) 0.052(4) 0.004(4) -0.002(4) 0.044(5) C21 0.065(5) 0.055(5) 0.052(4) 0.004(3) 0.007(4) 0.016(4) C22 0.063(5) 0.074(5) 0.045(4) -0.001(4) 0.001(3) 0.025(4) C23 0.067(6) 0.103(7) 0.079(6) -0.007(5) -0.016(4) 0.031(6) C24 0.065(6) 0.149(10) 0.071(5) -0.004(6) 0.001(4) 0.055(7) C25 0.107(9) 0.135(10) 0.066(5) -0.008(6) -0.006(6) 0.084(8) C26 0.100(7) 0.093(6) 0.056(5) -0.011(4) -0.009(5) 0.059(6) Cl1 0.0924(17) 0.107(3) 0.086(2) 0.0011(19) 0.0006(9) 0.0535(13) O11 0.186(10) 0.156(9) 0.156(8) 0.025(6) -0.020(7) 0.110(8) O12 0.151(8) 0.184(9) 0.136(6) 0.008(6) 0.018(5) 0.126(7) Cl2 0.078(2) 0.0859(18) 0.082(2) 0.0017(8) 0.0033(16) 0.0389(10) N7 0.078(2) 0.0859(18) 0.082(2) 0.0017(8) 0.0033(16) 0.0389(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.251(7) . ? Ag1 N6 2.266(6) 4 ? Ag1 N5 2.401(6) 4 ? Ag1 N2 2.453(6) . ? N1 C1 1.319(11) . ? N1 C5 1.326(10) . ? N2 C6 1.255(10) . ? N2 N3 1.417(8) . ? N3 C7 1.270(9) . ? N4 C14 1.256(9) . ? N4 N5 1.397(9) . ? N5 C21 1.284(10) . ? N5 Ag1 2.401(6) 4 ? N6 C26 1.312(11) . ? N6 C22 1.392(11) . ? N6 Ag1 2.266(6) 4 ? C1 C2 1.369(15) . ? C1 H1A 0.9300 . ? C2 C3 1.343(17) . ? C2 H2A 0.9300 . ? C3 C4 1.364(16) . ? C3 H3B 0.9300 . ? C4 C5 1.366(13) . ? C4 H4B 0.9300 . ? C5 C6 1.446(11) . ? C6 H6B 0.9300 . ? C7 C8 1.477(9) . ? C7 C14 1.517(10) . ? C8 C9 1.369(12) . ? C8 C13 1.371(11) . ? C9 C10 1.392(12) . ? C9 H9A 0.9300 . ? C10 C11 1.360(14) . ? C10 H10A 0.9300 . ? C11 C12 1.342(14) . ? C11 H11A 0.9300 . ? C12 C13 1.357(12) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.476(11) . ? C15 C16 1.398(12) . ? C15 C20 1.419(11) . ? C16 C17 1.359(13) . ? C16 H16A 0.9300 . ? C17 C18 1.315(15) . ? C17 H17A 0.9300 . ? C18 C19 1.413(16) . ? C18 H18A 0.9300 . ? C19 C20 1.345(12) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.429(11) . ? C21 H21A 0.9300 . ? C22 C23 1.354(12) . ? C23 C24 1.403(15) . ? C23 H23A 0.9300 . ? C24 C25 1.322(15) . ? C24 H24A 0.9300 . ? C25 C26 1.416(14) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? Cl1 O11 1.385(8) 5 ? Cl1 O11 1.385(8) . ? Cl1 O12 1.409(9) 5 ? Cl1 O12 1.409(8) . ? Cl2 O24 1.427(11) 6_554 ? Cl2 O24 1.427(11) . ? Cl2 O22 1.431(11) . ? Cl2 O22 1.431(11) 6_554 ? Cl2 O23 1.460(12) . ? Cl2 O23 1.460(12) 6_554 ? Cl2 O21 1.475(12) . ? O22 O24 1.19(2) 6_554 ? O22 O23 1.53(2) 6_554 ? O23 O24 1.46(2) 6_554 ? O23 O22 1.53(2) 6_554 ? O24 O22 1.19(2) 6_554 ? O24 O23 1.46(2) 6_554 ? O21' O23' 0.68(4) 6_554 ? O22' O22' 1.23(6) 6_554 ? O23' O21' 0.68(4) 6_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N6 127.2(3) . 4 ? N1 Ag1 N5 140.8(2) . 4 ? N6 Ag1 N5 73.4(3) 4 4 ? N1 Ag1 N2 72.1(2) . . ? N6 Ag1 N2 122.7(2) 4 . ? N5 Ag1 N2 129.0(2) 4 . ? C1 N1 C5 117.9(8) . . ? C1 N1 Ag1 125.4(6) . . ? C5 N1 Ag1 116.5(5) . . ? C6 N2 N3 111.2(6) . . ? C6 N2 Ag1 109.0(5) . . ? N3 N2 Ag1 139.7(5) . . ? C7 N3 N2 115.9(6) . . ? C14 N4 N5 116.3(6) . . ? C21 N5 N4 113.9(6) . . ? C21 N5 Ag1 109.9(5) . 4 ? N4 N5 Ag1 132.0(5) . 4 ? C26 N6 C22 117.6(7) . . ? C26 N6 Ag1 128.8(6) . 4 ? C22 N6 Ag1 113.6(5) . 4 ? N1 C1 C2 121.5(10) . . ? N1 C1 H1A 119.3 . . ? C2 C1 H1A 119.3 . . ? C3 C2 C1 121.2(11) . . ? C3 C2 H2A 119.4 . . ? C1 C2 H2A 119.4 . . ? C2 C3 C4 117.1(12) . . ? C2 C3 H3B 121.4 . . ? C4 C3 H3B 121.4 . . ? C3 C4 C5 119.7(12) . . ? C3 C4 H4B 120.1 . . ? C5 C4 H4B 120.1 . . ? N1 C5 C4 122.5(10) . . ? N1 C5 C6 117.7(7) . . ? C4 C5 C6 119.8(9) . . ? N2 C6 C5 124.3(7) . . ? N2 C6 H6B 117.8 . . ? C5 C6 H6B 117.8 . . ? N3 C7 C8 118.5(6) . . ? N3 C7 C14 125.4(6) . . ? C8 C7 C14 116.0(6) . . ? C9 C8 C13 119.0(7) . . ? C9 C8 C7 120.5(7) . . ? C13 C8 C7 120.5(7) . . ? C8 C9 C10 119.8(9) . . ? C8 C9 H9A 120.1 . . ? C10 C9 H9A 120.1 . . ? C11 C10 C9 118.4(10) . . ? C11 C10 H10A 120.8 . . ? C9 C10 H10A 120.8 . . ? C12 C11 C10 122.6(9) . . ? C12 C11 H11A 118.7 . . ? C10 C11 H11A 118.7 . . ? C11 C12 C13 118.6(9) . . ? C11 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? C12 C13 C8 121.7(9) . . ? C12 C13 H13A 119.2 . . ? C8 C13 H13A 119.2 . . ? N4 C14 C15 118.8(7) . . ? N4 C14 C7 124.7(7) . . ? C15 C14 C7 116.1(7) . . ? C16 C15 C20 117.0(8) . . ? C16 C15 C14 122.7(8) . . ? C20 C15 C14 120.3(8) . . ? C17 C16 C15 119.4(9) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C18 C17 C16 121.9(11) . . ? C18 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C17 C18 C19 122.5(9) . . ? C17 C18 H18A 118.8 . . ? C19 C18 H18A 118.8 . . ? C20 C19 C18 116.0(10) . . ? C20 C19 H19A 122.0 . . ? C18 C19 H19A 122.0 . . ? C19 C20 C15 123.2(10) . . ? C19 C20 H20A 118.4 . . ? C15 C20 H20A 118.4 . . ? N5 C21 C22 123.0(7) . . ? N5 C21 H21A 118.5 . . ? C22 C21 H21A 118.5 . . ? C23 C22 N6 120.0(8) . . ? C23 C22 C21 121.8(8) . . ? N6 C22 C21 118.1(7) . . ? C22 C23 C24 121.7(10) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C25 C24 C23 117.5(9) . . ? C25 C24 H24A 121.2 . . ? C23 C24 H24A 121.2 . . ? C24 C25 C26 119.9(10) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? N6 C26 C25 123.0(10) . . ? N6 C26 H26A 118.5 . . ? C25 C26 H26A 118.5 . . ? O11 Cl1 O11 108.6(10) 5 . ? O11 Cl1 O12 109.8(6) 5 5 ? O11 Cl1 O12 110.2(6) . 5 ? O11 Cl1 O12 110.2(6) 5 . ? O11 Cl1 O12 109.8(6) . . ? O12 Cl1 O12 108.3(8) 5 . ? O24 Cl2 O24 141.1(14) 6_554 . ? O24 Cl2 O22 49.3(8) 6_554 . ? O24 Cl2 O22 115.6(8) . . ? O24 Cl2 O22 115.6(8) 6_554 6_554 ? O24 Cl2 O22 49.3(8) . 6_554 ? O22 Cl2 O22 141.3(14) . 6_554 ? O24 Cl2 O23 60.6(8) 6_554 . ? O24 Cl2 O23 112.5(8) . . ? O22 Cl2 O23 109.4(8) . . ? O22 Cl2 O23 63.9(8) 6_554 . ? O24 Cl2 O23 112.5(8) 6_554 6_554 ? O24 Cl2 O23 60.6(8) . 6_554 ? O22 Cl2 O23 63.9(8) . 6_554 ? O22 Cl2 O23 109.4(8) 6_554 6_554 ? O23 Cl2 O23 161.4(13) . 6_554 ? O24 Cl2 O21 109.5(7) 6_554 . ? O24 Cl2 O21 109.5(7) . . ? O22 Cl2 O21 109.4(7) . . ? O22 Cl2 O21 109.4(7) 6_554 . ? O23 Cl2 O21 99.3(7) . . ? O23 Cl2 O21 99.3(7) 6_554 . ? O24 O22 Cl2 65.2(6) 6_554 . ? O24 O22 O23 123.3(9) 6_554 6_554 ? Cl2 O22 O23 59.0(5) . 6_554 ? O24 O23 Cl2 58.6(5) 6_554 . ? O24 O23 O22 108.0(10) 6_554 6_554 ? Cl2 O23 O22 57.1(5) . 6_554 ? O22 O24 Cl2 65.5(6) 6_554 . ? O22 O24 O23 125.6(9) 6_554 6_554 ? Cl2 O24 O23 60.8(5) . 6_554 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.731 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.102