# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 898413' #TrackingRef 'CCDC-898413.cif' _audit_creation_date 2011-05-14T23:59:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'C52 H40 Ag2 Cl6 N4 O6' _chemical_formula_moiety 'C52 H40 Ag2 Cl6 N4 O6' _chemical_formula_weight 1245.32 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _cell_length_a 8.7777(10) _cell_length_b 10.8623(12) _cell_length_c 14.2447(15) _cell_angle_alpha 101.878(5) _cell_angle_beta 104.271(5) _cell_angle_gamma 98.735(5) _cell_volume 1258.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _cell_measurement_reflns_used 5491 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.7618 _exptl_absorpt_correction_T_max 0.8936 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_unetI/netI 0.0252 _diffrn_reflns_number 8265 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD phi and omega scans' _diffrn_detector_area_resol_mean 9 _reflns_number_total 4417 _reflns_number_gt 3623 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae, 2008)' _computing_publication_material 'WinGX (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. Numerous constraints and restraints were utilised to model the thermal disorder of the chlorate anion. Specifically, the EADP constraint was used to make the anisotropic displacement parameters of Cl3a, O1a, O2a and O3a equal to those of Cl3b, O1b, O2b and O3b. The ISOR command was utilised to restrain the anisotropic U-values of the atoms O1a, O2a, O3a, O1b, O2b, O3b, O1c, O2c, O3c, Cl3a, Cl3b, Cl3c to behave more isotropically. The SIMU/DELU restraints were used to make the ADP values of the atoms Ag1, O1C, O3a, O3b, O3c, C10, C11 and C12 more reasonable. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.2700P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4417 _refine_ls_number_parameters 329 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.042 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.61 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.051 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 -0.3045(3) 0.5645(2) 0.8978(2) 0.0527(6) Uani 1 1 d . . . C2 C -0.4574(4) 0.4923(3) 0.8523(2) 0.0631(7) Uani 1 1 d . A . C3 C -0.5372(3) 0.5052(3) 0.7602(2) 0.0633(7) Uani 1 1 d . . . C4 C -0.4637(3) 0.5904(2) 0.7154(2) 0.0536(6) Uani 1 1 d . A . C5 C -0.3095(3) 0.6595(3) 0.7695(2) 0.0531(6) Uani 1 1 d . . . C6 C -0.5385(4) 0.6119(3) 0.6183(2) 0.0625(7) Uani 1 1 d . . . C7 C -0.6779(3) 0.5487(3) 0.5540(2) 0.0616(7) Uani 1 1 d . A . C8 C -0.7525(3) 0.5701(3) 0.4569(2) 0.0584(7) Uani 1 1 d . . . C9 C -0.8967(4) 0.4912(3) 0.3959(2) 0.0644(7) Uani 1 1 d . . . C10 C -0.9692(4) 0.5100(3) 0.3042(2) 0.0735(8) Uani 1 1 d . . . C11 C -0.8997(4) 0.6069(3) 0.2707(2) 0.0701(8) Uani 1 1 d . . . C12 C -0.7572(5) 0.6863(4) 0.3295(3) 0.0827(10) Uani 1 1 d . . . C13 C -0.6836(4) 0.6688(3) 0.4210(3) 0.0791(9) Uani 1 1 d . . . C14 C 0.3427(3) 0.8259(2) 0.8842(2) 0.0537(6) Uani 1 1 d . . . C15 C 0.5061(3) 0.8581(2) 0.8974(2) 0.0581(7) Uani 1 1 d . A . C16 C 0.6067(3) 0.8594(3) 0.9877(2) 0.0584(7) Uani 1 1 d . . . C17 C 0.5451(3) 0.8306(2) 1.0640(2) 0.0507(6) Uani 1 1 d . A . C18 C 0.3782(3) 0.8000(2) 1.0418(2) 0.0514(6) Uani 1 1 d . . . C19 C 0.6499(3) 0.8344(3) 1.1618(2) 0.0578(7) Uani 1 1 d . . . C20 C 0.6110(3) 0.8614(3) 1.2474(2) 0.0590(7) Uani 1 1 d . A . C21 C 0.7078(3) 0.8636(3) 1.3471(2) 0.0583(7) Uani 1 1 d . . . C22 C 0.8444(4) 0.8138(3) 1.3646(3) 0.0709(8) Uani 1 1 d . A . C23 C 0.9297(5) 0.8147(3) 1.4609(3) 0.0865(10) Uani 1 1 d . . . C24 C 0.8777(5) 0.8661(4) 1.5414(3) 0.0904(11) Uani 1 1 d . A . C25 C 0.7440(5) 0.9161(4) 1.5257(3) 0.0937(11) Uani 1 1 d . . . C26 C 0.6593(4) 0.9159(3) 1.4298(2) 0.0783(9) Uani 1 1 d . A . H2 H -0.5058 0.4362 0.883 0.076 Uiso 1 1 calc R . . H3 H -0.6408 0.4568 0.7276 0.076 Uiso 1 1 calc R A . H5 H -0.2582 0.7174 0.7414 0.064 Uiso 1 1 calc R A . H6 H -0.4815 0.6775 0.5996 0.075 Uiso 1 1 calc R A . H7 H -0.7351 0.4832 0.5727 0.074 Uiso 1 1 calc R . . H9 H -0.9454 0.4242 0.4172 0.077 Uiso 1 1 calc R . . H10 H -1.0666 0.4562 0.2647 0.088 Uiso 1 1 calc R . . H11 H -0.9488 0.6188 0.2085 0.084 Uiso 1 1 calc R . . H12 H -0.7097 0.7528 0.3072 0.099 Uiso 1 1 calc R . . H13 H -0.5863 0.7233 0.4598 0.095 Uiso 1 1 calc R . . H15 H 0.5464 0.8781 0.8465 0.07 Uiso 1 1 calc R . . H16 H 0.7174 0.8798 0.9985 0.07 Uiso 1 1 calc R A . H18 H 0.3342 0.7795 1.0912 0.062 Uiso 1 1 calc R A . H19 H 0.7512 0.8167 1.1648 0.069 Uiso 1 1 calc R A . H20 H 0.5104 0.8811 1.243 0.071 Uiso 1 1 calc R . . H22 H 0.8801 0.7788 1.3108 0.085 Uiso 1 1 calc R . . H23 H 1.0218 0.7808 1.4712 0.104 Uiso 1 1 calc R A . H24 H 0.9341 0.8664 1.6059 0.108 Uiso 1 1 calc R . . H25 H 0.7088 0.9508 1.5798 0.112 Uiso 1 1 calc R A . H26 H 0.5684 0.9513 1.4204 0.094 Uiso 1 1 calc R . . Ag1 Ag 0.01393(2) 0.77715(2) 0.940917(18) 0.07243(12) Uani 1 1 d . . . Cl1 Cl -0.19848(10) 0.54884(8) 1.01309(6) 0.0763(2) Uani 1 1 d . A . Cl2 Cl 0.20939(11) 0.82104(8) 0.77060(6) 0.0781(2) Uani 1 1 d . A . Cl3A Cl 0.09939(9) 0.96343(7) 1.18438(7) 0.0589(3) Uani 0.940(2) 1 d PD A 1 Cl3B Cl 0.1366(15) 0.9766(13) 1.1421(11) 0.0589(3) Uani 0.060(2) 1 d PD A 2 N1 N -0.2297(2) 0.6481(2) 0.85946(16) 0.0503(5) Uani 1 1 d . A . N2 N 0.2774(2) 0.7981(2) 0.95430(16) 0.0513(5) Uani 1 1 d . A . O1A O 0.0504(4) 0.8295(2) 1.1311(2) 0.0958(10) Uani 0.940(2) 1 d PD A 1 O1B O 0.028(5) 0.854(3) 1.092(3) 0.0958(10) Uani 0.060(2) 1 d PD A 2 O2A O 0.2722(3) 0.9928(4) 1.2327(2) 0.1040(11) Uani 0.940(2) 1 d PD A 1 O2B O 0.239(5) 0.966(5) 1.236(3) 0.1040(11) Uani 0.060(2) 1 d PD A 2 O3A O 0.0839(6) 1.0305(4) 1.1028(3) 0.1454(15) Uani 0.940(2) 1 d PD . 1 O3B O 0.029(5) 1.059(4) 1.175(4) 0.1454(15) Uani 0.060(2) 1 d PD A 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 C1 0.0503(15) 0.0455(14) 0.0592(15) 0.0096(11) 0.0148(12) 0.0081(11) C2 0.0586(17) 0.0564(16) 0.0705(17) 0.0207(14) 0.0177(14) -0.0038(13) C3 0.0511(16) 0.0572(16) 0.0678(17) 0.0116(13) 0.0064(13) -0.0058(13) C4 0.0495(15) 0.0492(15) 0.0587(15) 0.0084(12) 0.0150(12) 0.0088(12) C5 0.0470(14) 0.0511(15) 0.0615(15) 0.0133(12) 0.0197(12) 0.0054(11) C6 0.0564(17) 0.0620(17) 0.0656(16) 0.0177(14) 0.0142(13) 0.0059(13) C7 0.0568(17) 0.0625(17) 0.0636(16) 0.0178(13) 0.0141(13) 0.0096(13) C8 0.0575(16) 0.0569(16) 0.0604(15) 0.0148(13) 0.0160(13) 0.0131(13) C9 0.0615(18) 0.0591(17) 0.0676(17) 0.0141(14) 0.0137(14) 0.0084(14) C10 0.067(2) 0.0658(19) 0.0725(19) 0.0064(16) 0.0030(16) 0.0138(15) C11 0.080(2) 0.072(2) 0.0620(17) 0.0215(15) 0.0156(16) 0.0304(17) C12 0.082(2) 0.085(2) 0.084(2) 0.0388(19) 0.0180(19) 0.0128(19) C13 0.067(2) 0.082(2) 0.079(2) 0.0315(17) 0.0046(16) -0.0014(16) C14 0.0561(16) 0.0383(13) 0.0658(16) 0.0100(12) 0.0206(13) 0.0068(11) C15 0.0607(17) 0.0437(14) 0.0757(18) 0.0097(13) 0.0360(15) 0.0092(12) C16 0.0446(14) 0.0482(15) 0.085(2) 0.0107(14) 0.0286(14) 0.0104(12) C17 0.0424(13) 0.0380(13) 0.0706(16) 0.0086(11) 0.0190(12) 0.0078(10) C18 0.0445(14) 0.0459(14) 0.0664(16) 0.0151(12) 0.0217(12) 0.0067(11) C19 0.0395(14) 0.0516(15) 0.0806(19) 0.0139(13) 0.0182(13) 0.0068(11) C20 0.0413(14) 0.0539(16) 0.0811(19) 0.0154(14) 0.0181(13) 0.0096(12) C21 0.0466(15) 0.0495(15) 0.0725(17) 0.0127(13) 0.0121(13) 0.0036(12) C22 0.0611(19) 0.0634(18) 0.086(2) 0.0205(16) 0.0168(16) 0.0125(15) C23 0.070(2) 0.076(2) 0.107(3) 0.027(2) 0.006(2) 0.0237(18) C24 0.088(3) 0.085(2) 0.082(2) 0.020(2) 0.001(2) 0.011(2) C25 0.086(3) 0.111(3) 0.074(2) 0.010(2) 0.0154(19) 0.020(2) C26 0.0628(19) 0.089(2) 0.078(2) 0.0121(18) 0.0159(16) 0.0187(17) Ag1 0.03994(14) 0.0903(2) 0.08352(19) 0.03405(14) 0.00981(11) 0.00023(11) Cl1 0.0710(5) 0.0764(5) 0.0714(5) 0.0277(4) 0.0034(4) 0.0014(4) Cl2 0.0823(5) 0.0741(5) 0.0711(5) 0.0242(4) 0.0139(4) 0.0022(4) Cl3A 0.0521(4) 0.0638(5) 0.0640(5) 0.0137(4) 0.0252(4) 0.0113(3) Cl3B 0.0521(4) 0.0638(5) 0.0640(5) 0.0137(4) 0.0252(4) 0.0113(3) N1 0.0409(11) 0.0478(12) 0.0602(12) 0.0085(10) 0.0166(10) 0.0070(9) N2 0.0404(11) 0.0459(12) 0.0670(13) 0.0149(10) 0.0174(10) 0.0034(9) O1A 0.115(2) 0.0626(15) 0.099(2) 0.0091(13) 0.0410(18) -0.0135(14) O1B 0.115(2) 0.0626(15) 0.099(2) 0.0091(13) 0.0410(18) -0.0135(14) O2A 0.0582(18) 0.147(3) 0.0853(16) 0.0101(17) 0.0114(13) -0.0014(17) O2B 0.0582(18) 0.147(3) 0.0853(16) 0.0101(17) 0.0114(13) -0.0014(17) O3A 0.188(4) 0.150(3) 0.161(3) 0.107(3) 0.071(3) 0.092(3) O3B 0.188(4) 0.150(3) 0.161(3) 0.107(3) 0.071(3) 0.092(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.371(4) . ? C2 C3 1.372(4) . ? C2 H2 0.93 . ? C3 H3 0.93 . ? C4 C3 1.395(4) . ? C4 C6 1.460(4) . ? C5 C4 1.389(4) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C6 1.319(4) . ? C7 H7 0.93 . ? C8 C13 1.400(4) . ? C8 C7 1.458(4) . ? C8 C9 1.383(4) . ? C9 H9 0.93 . ? C10 C9 1.375(4) . ? C10 H10 0.93 . ? C11 C10 1.365(5) . ? C11 C12 1.367(5) . ? C11 H11 0.93 . ? C12 C13 1.370(5) . ? C12 H12 0.93 . ? C13 H13 0.93 . ? C14 C15 1.379(4) . ? C15 H15 0.93 . ? C16 C15 1.364(4) . ? C16 H16 0.93 . ? C17 C16 1.396(4) . ? C18 C17 1.392(4) . ? C18 H18 0.93 . ? C19 C17 1.457(4) . ? C19 H19 0.93 . ? C20 C19 1.334(4) . ? C20 C21 1.458(4) . ? C20 H20 0.93 . ? C21 C22 1.378(4) . ? C21 C26 1.390(4) . ? C22 C23 1.389(5) . ? C22 H22 0.93 . ? C23 H23 0.93 . ? C24 C23 1.381(5) . ? C24 C25 1.355(5) . ? C24 H24 0.93 . ? C25 H25 0.93 . ? C26 C25 1.384(5) . ? C26 H26 0.93 . ? Ag1 N1 2.254(2) . ? Ag1 N2 2.245(2) . ? Ag1 O3A 2.511(3) 2_577 ? Cl1 C1 1.733(3) . ? Cl2 C14 1.733(3) . ? Cl3A O1A 1.439(3) . ? Cl3A O2A 1.458(3) . ? Cl3A O3A 1.483(3) . ? Cl3B O1B 1.440(3) . ? Cl3B O2B 1.458(4) . ? Cl3B O3B 1.483(4) . ? N1 C1 1.324(3) . ? N1 C5 1.341(3) . ? N2 C14 1.331(3) . ? N2 C18 1.334(3) . ? O1A Ag1 2.578(3) . ? O1B Ag1 2.11(5) . ? O3A Ag1 2.511(3) 2_577 ? 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 C1 C2 C3 118.1(3) . . ? C1 C2 H2 120.9 . . ? C1 N1 Ag1 123.54(18) . . ? C1 N1 C5 116.9(2) . . ? C2 C1 Cl1 119.5(2) . . ? C2 C3 C4 120.3(3) . . ? C2 C3 H3 119.8 . . ? C3 C2 H2 120.9 . . ? C3 C4 C6 124.6(2) . . ? C4 C3 H3 119.8 . . ? C4 C5 H5 117.8 . . ? C4 C6 H6 116.3 . . ? C5 C4 C3 116.2(3) . . ? C5 C4 C6 119.2(2) . . ? C5 N1 Ag1 119.48(17) . . ? C6 C7 C8 127.3(3) . . ? C6 C7 H7 116.3 . . ? C7 C6 C4 127.3(3) . . ? C7 C6 H6 116.3 . . ? C8 C13 H13 119.5 . . ? C8 C7 H7 116.3 . . ? C8 C9 H9 119.4 . . ? C9 C10 H10 119.7 . . ? C9 C8 C13 117.1(3) . . ? C9 C8 C7 120.3(3) . . ? C10 C11 C12 119.4(3) . . ? C10 C11 H11 120.3 . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 120.7(3) . . ? C11 C10 H10 119.7 . . ? C11 C12 C13 120.6(3) . . ? C11 C12 H12 119.7 . . ? C12 C11 H11 120.3 . . ? C12 C13 C8 121.0(3) . . ? C12 C13 H13 119.5 . . ? C13 C12 H12 119.7 . . ? C13 C8 C7 122.6(3) . . ? C14 C15 H15 121.2 . . ? C14 N2 Ag1 123.65(18) . . ? C14 N2 C18 117.0(2) . . ? C15 C14 Cl2 119.7(2) . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16 119.6 . . ? C16 C15 C14 117.7(3) . . ? C16 C15 H15 121.2 . . ? C16 C17 C19 121.8(2) . . ? C17 C16 H16 119.6 . . ? C17 C18 H18 118 . . ? C17 C19 H19 117.7 . . ? C18 C17 C16 116.3(3) . . ? C18 C17 C19 121.9(2) . . ? C18 N2 Ag1 118.73(16) . . ? C19 C20 C21 127.5(3) . . ? C19 C20 H20 116.2 . . ? C20 C19 C17 124.6(3) . . ? C20 C19 H19 117.7 . . ? C21 C20 H20 116.2 . . ? C21 C22 C23 121.3(3) . . ? C21 C22 H22 119.4 . . ? C21 C26 H26 119.4 . . ? C22 C21 C20 123.5(3) . . ? C22 C21 C26 117.4(3) . . ? C22 C23 H23 120 . . ? C23 C22 H22 119.4 . . ? C23 C24 H24 120.2 . . ? C24 C23 C22 119.9(3) . . ? C24 C23 H23 120 . . ? C24 C25 C26 120.6(4) . . ? C24 C25 H25 119.7 . . ? C25 C24 C23 119.6(4) . . ? C25 C24 H24 120.2 . . ? C25 C26 C21 121.2(3) . . ? C25 C26 H26 119.4 . . ? C26 C21 C20 119.0(3) . . ? C26 C25 H25 119.7 . . ? Cl3A O1A Ag1 116.67(16) . . ? Cl3A O3A Ag1 139.4(2) . 2_577 ? Cl3B O1B Ag1 117(3) . . ? N1 Ag1 O1A 109.45(8) . . ? N1 Ag1 O3A 91.28(13) . 2_577 ? N1 C1 C2 124.2(3) . . ? N1 C1 Cl1 116.36(19) . . ? N1 C5 C4 124.3(2) . . ? N1 C5 H5 117.8 . . ? N2 Ag1 N1 143.12(8) . . ? N2 Ag1 O1A 95.28(10) . . ? N2 Ag1 O3A 110.68(12) . 2_577 ? N2 C14 C15 124.2(3) . . ? N2 C14 Cl2 116.2(2) . . ? N2 C18 C17 124.1(2) . . ? N2 C18 H18 118 . . ? O1A Cl3A O2A 108.6(2) . . ? O1A Cl3A O3A 103.1(2) . . ? O1B Ag1 N1 110.3(10) . . ? O1B Ag1 N2 99.4(12) . . ? O1B Ag1 O1A 11.6(13) . . ? O1B Ag1 O3A 89.7(13) . 2_577 ? O1B Cl3B O2B 108.6(3) . . ? O1B Cl3B O3B 103.1(3) . . ? O2A Cl3A O3A 103.5(3) . . ? O2B Cl3B O3B 103.5(3) . . ? O3A Ag1 O1A 101.33(12) 2_577 . ? data_2 _database_code_depnum_ccdc_archive 'CCDC 898414' #TrackingRef 'CCDC-898414.cif' _audit_creation_date 2011-05-14T23:56:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'C52 H40 Ag2 Cl6 N4 O6' _chemical_formula_moiety 'C52 H40 Ag2 Cl6 N4 O6' _chemical_formula_weight 1245.32 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _cell_length_a 8.9589(10) _cell_length_b 11.5427(13) _cell_length_c 13.4841(14) _cell_angle_alpha 97.692(7) _cell_angle_beta 102.484(6) _cell_angle_gamma 103.767(5) _cell_volume 1296.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.35 _cell_measurement_reflns_used 4217 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.117 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.6860 _exptl_absorpt_correction_T_max 0.8965 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_unetI/netI 0.0429 _diffrn_reflns_number 7008 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD phi and omega scans' _diffrn_detector_area_resol_mean 9 _reflns_number_total 4480 _reflns_number_gt 2672 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo, Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL (Sheldrick, 2008)' _computing_molecular_graphics 'Mercury (Macrae, 2008)' _computing_publication_material 'WinGX (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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 EADP constraint in SHELX was used to make the anisotropic displacement parameters of Cl3a, O1a, O2a and O3a equal to those of Cl3b, O1b, O2b and O3b. ; _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^)+(0.0766P)^2^+1.4130P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4480 _refine_ls_number_parameters 365 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1153 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1616 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.664 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.632 _refine_diff_density_min -0.49 _refine_diff_density_rms 0.065 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.1844(13) 0.0754(10) 0.3845(8) 0.091(3) Uani 1 1 d . . . C2 C 0.0473(16) -0.0103(11) 0.3320(9) 0.122(5) Uani 1 1 d . B . C3 C -0.0106(14) -0.0116(10) 0.2292(9) 0.110(4) Uani 1 1 d . . . C4 C 0.0647(10) 0.0741(8) 0.1807(7) 0.071(2) Uani 1 1 d . B . C5 C 0.1964(10) 0.1613(8) 0.2444(7) 0.074(2) Uani 1 1 d . . . C6 C 0.0255(10) 0.0743(8) 0.0677(7) 0.074(2) Uani 1 1 d . . . C7 C -0.1299(10) -0.0173(8) -0.0049(7) 0.076(2) Uani 1 1 d . . . C8 C -0.2524(11) 0.0309(10) -0.0656(7) 0.083(3) Uani 1 1 d . . . C9 C -0.4076(12) -0.0403(12) -0.0991(9) 0.109(4) Uani 1 1 d . . . C10 C -0.5220(16) -0.0073(15) -0.1673(12) 0.137(5) Uani 1 1 d U . . C11 C -0.484(2) 0.0976(16) -0.2003(11) 0.143(5) Uani 1 1 d U . . C12 C -0.333(2) 0.1709(18) -0.1699(13) 0.153(5) Uani 1 1 d U . . C13 C -0.2177(15) 0.1347(13) -0.1034(11) 0.122(4) Uani 1 1 d . . . C14 C 0.8146(12) 0.3325(9) 0.3618(8) 0.083(3) Uani 1 1 d . . . C15 C 0.9729(12) 0.3535(9) 0.3701(8) 0.086(3) Uani 1 1 d . B . C16 C 1.0688(11) 0.3547(9) 0.4644(9) 0.085(3) Uani 1 1 d . . . C17 C 1.0060(10) 0.3333(9) 0.5477(8) 0.080(3) Uani 1 1 d . B . C18 C 0.8421(11) 0.3106(9) 0.5286(8) 0.087(3) Uani 1 1 d . . . C19 C 1.1063(11) 0.3380(9) 0.6491(8) 0.083(3) Uani 1 1 d . . . C20 C 1.0693(12) 0.3566(9) 0.7378(9) 0.085(3) Uani 1 1 d . B . C21 C 1.1675(11) 0.3632(9) 0.8415(8) 0.083(3) Uani 1 1 d . . . C22 C 1.3078(12) 0.3296(9) 0.8583(8) 0.087(3) Uani 1 1 d . . . C23 C 1.3954(13) 0.3353(11) 0.9569(10) 0.102(3) Uani 1 1 d . . . C24 C 1.3457(16) 0.3759(11) 1.0401(10) 0.104(4) Uani 1 1 d . . . C25 C 1.2102(17) 0.4089(12) 1.0264(9) 0.112(4) Uani 1 1 d . . . C26 C 1.1196(14) 0.4018(11) 0.9274(9) 0.104(3) Uani 1 1 d . . . Ag1 Ag 0.48933(9) 0.30357(9) 0.43261(7) 0.1127(5) Uani 1 1 d U . . Cl1 Cl 0.2706(5) 0.0757(3) 0.5124(2) 0.1345(13) Uani 1 1 d . B . Cl2 Cl 0.6873(4) 0.3334(3) 0.2451(2) 0.1162(11) Uani 1 1 d . B . Cl3A Cl 0.5612(12) 0.4583(10) 0.6765(8) 0.0776(19) Uani 0.432(6) 1 d PDU A 1 Cl3B Cl 0.5823(13) 0.4466(10) 0.6963(9) 0.0776(19) Uani 0.398(10) 1 d PDU B 2 Cl3C Cl 0.614(3) 0.461(3) 0.642(2) 0.149 Uiso 0.169(9) 1 d PD B 3 H2 H -0.0056 -0.0664 0.365 0.146 Uiso 1 1 calc R . . H3 H -0.1023 -0.0712 0.1913 0.132 Uiso 1 1 calc R B . H5 H 0.246 0.2237 0.2156 0.088 Uiso 1 1 calc R B . H6 H 0.0303 0.157 0.0563 0.089 Uiso 1 1 calc R . . H7 H -0.1787 -0.0756 0.0333 0.091 Uiso 1 1 calc R . . H9 H -0.4362 -0.1123 -0.0752 0.131 Uiso 1 1 calc R . . H10 H -0.6254 -0.0579 -0.1903 0.164 Uiso 1 1 calc R . . H11 H -0.5618 0.1204 -0.2446 0.171 Uiso 1 1 calc R . . H12 H -0.3065 0.2437 -0.1929 0.183 Uiso 1 1 calc R . . H13 H -0.1133 0.1836 -0.0841 0.146 Uiso 1 1 calc R . . H15 H 1.0146 0.3666 0.3138 0.104 Uiso 1 1 calc R . . H16 H 1.1779 0.3701 0.4727 0.102 Uiso 1 1 calc R B . H18 H 0.7957 0.2943 0.5825 0.105 Uiso 1 1 calc R B . H19 H 1.2064 0.3269 0.6515 0.1 Uiso 1 1 calc R B . H20 H 0.9684 0.3666 0.7344 0.102 Uiso 1 1 calc R . . H22 H 1.3435 0.3027 0.8019 0.105 Uiso 1 1 calc R . . H23 H 1.4887 0.3113 0.9667 0.122 Uiso 1 1 calc R . . H24 H 1.406 0.3808 1.1068 0.125 Uiso 1 1 calc R . . H25 H 1.1769 0.4368 1.0835 0.134 Uiso 1 1 calc R . . H26 H 1.0247 0.4234 0.9189 0.125 Uiso 1 1 calc R . . N1 N 0.2585(8) 0.1629(7) 0.3452(6) 0.076(2) Uani 1 1 d . B . N2 N 0.7469(8) 0.3108(7) 0.4375(7) 0.083(2) Uani 1 1 d . B . O1A O 0.735(2) 0.517(2) 0.7112(18) 0.136(6) Uani 0.432(6) 1 d PDU A 1 O1B O 0.647(3) 0.5642(16) 0.6665(18) 0.136(6) Uani 0.398(10) 1 d PDU . 2 O1C O 0.532(5) 0.541(4) 0.692(4) 0.1201(13) Uani 0.169(9) 1 d PDU B 3 O2A O 0.568(3) 0.3338(19) 0.6649(19) 0.151(7) Uani 0.432(6) 1 d PDU A 1 O2B O 0.732(3) 0.421(3) 0.734(2) 0.151(7) Uani 0.398(10) 1 d PDU B 2 O2C O 0.756(6) 0.489(6) 0.727(6) 0.185(4) Uani 0.169(9) 1 d PDU B 3 O3A O 0.476(2) 0.470(2) 0.5798(15) 0.146(8) Uani 0.432(6) 1 d PDU . 1 O3B O 0.489(2) 0.3466(17) 0.6185(18) 0.121(4) Uani 0.398(10) 1 d PDU B 2 O3C O 0.550(7) 0.335(3) 0.624(4) 0.105(4) Uani 0.169(9) 1 d PDU B 3 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 0.089(7) 0.095(7) 0.067(6) 0.009(5) 0.005(5) 0.003(6) C2 0.147(11) 0.103(8) 0.069(7) 0.015(6) 0.012(7) -0.036(8) C3 0.106(8) 0.096(8) 0.082(8) 0.005(6) 0.005(6) -0.034(6) C4 0.062(5) 0.062(5) 0.072(6) 0.002(4) 0.003(4) 0.004(4) C5 0.061(5) 0.073(6) 0.074(6) 0.011(5) 0.007(4) 0.005(4) C6 0.064(5) 0.064(5) 0.075(6) 0.012(4) -0.002(4) -0.002(4) C7 0.056(5) 0.080(6) 0.075(6) 0.014(5) -0.002(4) 0.005(4) C8 0.067(6) 0.099(8) 0.072(6) 0.013(5) 0.004(5) 0.020(5) C9 0.068(7) 0.115(9) 0.114(9) -0.016(7) -0.013(6) 0.018(6) C10 0.089(8) 0.140(11) 0.147(13) -0.028(9) -0.032(8) 0.054(8) C11 0.145(9) 0.171(13) 0.107(10) -0.003(9) -0.020(9) 0.096(10) C12 0.153(11) 0.181(14) 0.153(14) 0.074(12) 0.032(11) 0.084(9) C13 0.091(8) 0.139(11) 0.140(11) 0.064(9) 0.012(8) 0.036(8) C14 0.071(6) 0.081(7) 0.081(7) 0.008(5) 0.004(5) 0.008(5) C15 0.073(6) 0.098(8) 0.086(7) 0.020(6) 0.020(5) 0.018(5) C16 0.058(5) 0.091(7) 0.100(8) 0.015(6) 0.014(5) 0.017(5) C17 0.058(5) 0.078(6) 0.091(7) 0.011(5) 0.007(5) 0.010(4) C18 0.065(6) 0.100(7) 0.082(7) 0.011(5) 0.013(5) 0.003(5) C19 0.058(5) 0.089(7) 0.094(8) 0.016(6) 0.008(5) 0.015(5) C20 0.066(6) 0.087(7) 0.097(8) 0.013(6) 0.013(5) 0.020(5) C21 0.064(6) 0.076(6) 0.093(7) 0.017(5) 0.006(5) 0.004(5) C22 0.075(6) 0.098(7) 0.081(7) 0.022(5) 0.011(5) 0.014(5) C23 0.076(7) 0.112(9) 0.111(9) 0.042(7) 0.011(7) 0.016(6) C24 0.092(8) 0.103(9) 0.101(9) 0.029(7) -0.001(7) 0.011(7) C25 0.119(10) 0.123(10) 0.082(8) 0.011(7) 0.013(7) 0.028(8) C26 0.092(8) 0.120(9) 0.095(9) 0.007(7) 0.014(7) 0.034(7) Ag1 0.0590(5) 0.1458(9) 0.1028(7) 0.0207(5) -0.0049(4) -0.0036(4) Cl1 0.148(3) 0.144(3) 0.0758(18) 0.0251(18) -0.0012(18) -0.003(2) Cl2 0.098(2) 0.128(2) 0.0904(19) 0.0247(17) -0.0121(15) 0.0012(17) Cl3A 0.070(2) 0.086(2) 0.071(3) 0.016(2) 0.016(2) 0.0136(17) Cl3B 0.070(2) 0.086(2) 0.071(3) 0.016(2) 0.016(2) 0.0136(17) N1 0.056(4) 0.088(5) 0.070(5) 0.006(4) 0.008(4) 0.006(4) N2 0.056(4) 0.090(6) 0.087(6) 0.014(4) 0.006(4) 0.004(4) O1A 0.133(7) 0.135(7) 0.137(7) 0.028(3) 0.037(4) 0.031(3) O1B 0.133(7) 0.135(7) 0.137(7) 0.028(3) 0.037(4) 0.031(3) O1C 0.12 0.120(2) 0.120(2) 0.0234(16) 0.0310(16) 0.0334(15) O2A 0.152(7) 0.151(7) 0.151(7) 0.032(3) 0.037(4) 0.043(4) O2B 0.152(7) 0.151(7) 0.151(7) 0.032(3) 0.037(4) 0.043(4) O2C 0.186 0.184(7) 0.185(7) 0.036(5) 0.048(5) 0.050(5) O3A 0.146(8) 0.146(8) 0.146(8) 0.028(2) 0.036(2) 0.042(3) O3B 0.117(7) 0.121(7) 0.122(3) 0.020(4) 0.035(5) 0.024(4) O3C 0.105(7) 0.104(7) 0.1053(19) 0.022(5) 0.025(5) 0.028(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C2 C1 1.359(15) . ? C2 C3 1.368(15) . ? C2 H2 0.93 . ? C3 H3 0.93 . ? C4 C3 1.381(13) . ? C4 C5 1.381(11) . ? C4 C6 1.488(13) . ? C5 H5 0.93 . ? C6 C7 1.565(11) . ? C6 C7 1.584(13) 2 ? C6 H6 0.98 . ? C7 C6 1.584(13) 2 ? C7 H7 0.98 . ? C8 C13 1.359(15) . ? C8 C7 1.485(13) . ? C8 C9 1.378(14) . ? C9 C10 1.384(17) . ? C9 H9 0.93 . ? C10 H10 0.93 . ? C11 C10 1.34(2) . ? C11 C12 1.35(2) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C12 1.396(18) . ? C13 H13 0.93 . ? C14 C15 1.357(14) . ? C14 Cl2 1.736(10) . ? C15 H15 0.93 . ? C16 C15 1.369(14) . ? C16 H16 0.93 . ? C17 C16 1.386(14) . ? C17 C19 1.451(13) . ? C18 C17 1.388(13) . ? C18 H18 0.93 . ? C19 H19 0.93 . ? C20 C19 1.313(13) . ? C20 H20 0.93 . ? C21 C20 1.463(14) . ? C21 C26 1.376(15) . ? C22 C21 1.384(14) . ? C22 H22 0.93 . ? C23 C22 1.374(15) . ? C23 C24 1.361(17) . ? C23 H23 0.93 . ? C24 H24 0.93 . ? C25 C24 1.339(17) . ? C25 C26 1.384(16) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? Ag1 N1 2.267(7) . ? Ag1 N2 2.276(8) . ? Ag1 O1B 2.52(2) 2_666 ? Ag1 O3A 2.59(2) 2_666 ? Ag1 O3B 2.49(2) . ? Ag1 O3C 2.47(6) . ? Cl1 C1 1.729(10) . ? Cl3A O1A 1.486(16) . ? Cl3A O2A 1.44(2) . ? Cl3A O3A 1.403(16) . ? Cl3B O1B 1.487(16) . ? Cl3B O2B 1.44(2) . ? Cl3B O3B 1.402(16) . ? Cl3C O1C 1.487(16) . ? Cl3C O2C 1.44(2) . ? Cl3C O3C 1.404(16) . ? N1 C1 1.311(12) . ? N1 C5 1.349(11) . ? N2 C14 1.318(12) . ? N2 C18 1.336(12) . ? O1B Ag1 2.52(2) 2_666 ? O3A Ag1 2.59(2) 2_666 ? 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 C1 C2 C3 118.1(10) . . ? C1 C2 H2 121 . . ? C1 N1 Ag1 123.9(6) . . ? C1 N1 C5 116.3(8) . . ? C2 C1 Cl1 120.3(9) . . ? C2 C3 C4 121.1(9) . . ? C2 C3 H3 119.4 . . ? C3 C2 H2 121 . . ? C3 C4 C6 126.3(8) . . ? C4 C3 H3 119.4 . . ? C4 C5 H5 117.5 . . ? C4 C6 C7 115.5(8) . 2 ? C4 C6 C7 119.4(8) . . ? C4 C6 H6 110 . . ? C5 C4 C3 115.0(9) . . ? C5 C4 C6 118.5(8) . . ? C5 N1 Ag1 119.6(6) . . ? C6 C7 C6 89.5(7) . 2 ? C6 C7 H7 110.2 . . ? C6 C7 H7 110.2 2 . ? C7 C6 C7 90.5(7) . 2 ? C7 C6 H6 110 . . ? C7 C6 H6 110 2 . ? C8 C13 C12 122.5(14) . . ? C8 C13 H13 118.7 . . ? C8 C7 C6 116.2(8) . 2 ? C8 C7 C6 119.1(8) . . ? C8 C7 H7 110.2 . . ? C8 C9 C10 121.5(14) . . ? C8 C9 H9 119.2 . . ? C9 C10 H10 120 . . ? C9 C8 C7 119.2(10) . . ? C10 C11 C12 120.9(14) . . ? C10 C11 H11 119.6 . . ? C10 C9 H9 119.2 . . ? C11 C10 C9 120.0(14) . . ? C11 C10 H10 120 . . ? C11 C12 C13 118.5(17) . . ? C11 C12 H12 120.8 . . ? C12 C11 H11 119.6 . . ? C12 C13 H13 118.7 . . ? C13 C12 H12 120.8 . . ? C13 C8 C7 123.6(9) . . ? C13 C8 C9 116.5(11) . . ? C14 C15 C16 117.5(10) . . ? C14 C15 H15 121.3 . . ? C14 N2 Ag1 124.9(7) . . ? C14 N2 C18 117.1(8) . . ? C15 C14 Cl2 119.7(9) . . ? C15 C16 C17 121.1(9) . . ? C15 C16 H16 119.4 . . ? C16 C15 H15 121.3 . . ? C16 C17 C18 115.8(9) . . ? C16 C17 C19 121.9(9) . . ? C17 C16 H16 119.4 . . ? C17 C18 H18 118.1 . . ? C17 C19 H19 116.9 . . ? C18 C17 C19 122.3(10) . . ? C18 N2 Ag1 117.3(7) . . ? C19 C20 C21 127.8(10) . . ? C19 C20 H20 116.1 . . ? C20 C19 C17 126.2(9) . . ? C20 C19 H19 116.9 . . ? C21 C20 H20 116.1 . . ? C21 C22 H22 119.4 . . ? C21 C26 C25 121.1(12) . . ? C21 C26 H26 119.4 . . ? C22 C21 C20 122.9(10) . . ? C22 C23 H23 120 . . ? C23 C22 C21 121.1(11) . . ? C23 C22 H22 119.4 . . ? C23 C24 H24 119.9 . . ? C24 C23 C22 120.1(11) . . ? C24 C23 H23 120 . . ? C24 C25 C26 120.3(13) . . ? C24 C25 H25 119.8 . . ? C25 C24 C23 120.2(12) . . ? C25 C24 H24 119.9 . . ? C25 C26 H26 119.4 . . ? C26 C21 C20 119.9(10) . . ? C26 C21 C22 117.2(10) . . ? C26 C25 H25 119.8 . . ? Cl3A O3A Ag1 111.2(12) . 2_666 ? Cl3B O1B Ag1 131.4(15) . 2_666 ? Cl3B O3B Ag1 129.0(12) . . ? Cl3C O3C Ag1 96(3) . . ? N1 Ag1 N2 131.3(3) . . ? N1 Ag1 O1B 80.5(5) . 2_666 ? N1 Ag1 O3A 119.7(5) . 2_666 ? N1 Ag1 O3B 108.3(5) . . ? N1 Ag1 O3C 115.9(11) . . ? N1 C1 C2 124.2(10) . . ? N1 C1 Cl1 115.5(7) . . ? N1 C5 C4 125.1(9) . . ? N1 C5 H5 117.5 . . ? N2 Ag1 O1B 120.5(6) . 2_666 ? N2 Ag1 O3A 94.4(5) . 2_666 ? N2 Ag1 O3B 103.8(6) . . ? N2 Ag1 O3C 90.9(13) . . ? N2 C14 C15 124.6(9) . . ? N2 C14 Cl2 115.7(7) . . ? N2 C18 C17 123.9(9) . . ? N2 C18 H18 118.1 . . ? O1B Ag1 O3A 39.6(7) 2_666 2_666 ? O2A Cl3A O1A 97.5(13) . . ? O2B Cl3B O1B 97.4(13) . . ? O2C Cl3C O1C 97.5(13) . . ? O3A Cl3A O1A 119.0(12) . . ? O3A Cl3A O2A 106.0(12) . . ? O3B Ag1 O1B 110.7(7) . 2_666 ? O3B Ag1 O3A 91.7(6) . 2_666 ? O3B Cl3B O1B 119.0(12) . . ? O3B Cl3B O2B 106.2(12) . . ? O3C Ag1 O1B 121.7(12) . 2_666 ? O3C Ag1 O3A 96.5(8) . 2_666 ? O3C Ag1 O3B 13.4(12) . . ? O3C Cl3C O1C 118.9(12) . . ? O3C Cl3C O2C 106.0(12) . . ?