# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_imw1536c2c _database_code_depnum_ccdc_archive 'CCDC 895598' #TrackingRef 'Ag_Ward_Stephenson_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H60 Ag3 Cl3 N20 O15' _chemical_formula_weight 1851.34 _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' Ag Ag -0.8971 1.1015 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.9323(11) _cell_length_b 15.4688(4) _cell_length_c 25.4156(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.234(2) _cell_angle_gamma 90.00 _cell_volume 14451.8(7) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9866 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.37 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7456 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7538 _exptl_absorpt_correction_T_max 0.9518 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 128797 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.46 _reflns_number_total 16509 _reflns_number_gt 12737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. There are three monomeric [Ag(C22H18N6O)][ClO4] structures in the asymmetric unit, as well as two acetonitrile solvent molecules. The H atoms were all added in calculated positions. All non-H atoms were made anisotropic. Two of the perchlorate anions suffered from disorder along one O > Cl bond (O12 > Cl11 47:53, and O22 > Cl21 52:48). 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^)+(0.0612P)^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_number_reflns 16509 _refine_ls_number_parameters 1058 _refine_ls_number_restraints 297 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _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 0.749904(6) 0.659477(15) 0.695488(9) 0.02374(7) Uani 1 1 d . . . Ag2 Ag 0.734176(6) 0.450603(15) 0.698037(9) 0.02653(7) Uani 1 1 d . . . Ag3 Ag 0.963597(7) 0.605085(15) 0.896454(10) 0.03039(7) Uani 1 1 d . . . N11A N 0.71249(6) 0.66631(15) 0.74584(9) 0.0212(5) Uani 1 1 d . . . C12A C 0.72288(8) 0.63407(19) 0.79795(11) 0.0230(6) Uani 1 1 d . . . H12A H 0.7465 0.6098 0.8128 0.028 Uiso 1 1 calc R . . C13A C 0.70096(8) 0.63455(19) 0.83083(12) 0.0259(6) Uani 1 1 d . . . H13A H 0.7092 0.6105 0.8673 0.031 Uiso 1 1 calc R . . C14A C 0.66665(9) 0.67091(19) 0.80950(12) 0.0266(7) Uani 1 1 d . . . H14A H 0.6508 0.6717 0.8309 0.032 Uiso 1 1 calc R . . C15A C 0.65585(8) 0.70610(19) 0.75650(12) 0.0256(6) Uani 1 1 d . . . H15A H 0.6326 0.7321 0.7414 0.031 Uiso 1 1 calc R . . C16A C 0.67936(8) 0.70314(18) 0.72550(11) 0.0208(6) Uani 1 1 d . . . N21A N 0.67585(6) 0.78758(15) 0.59448(9) 0.0211(5) Uani 1 1 d . . . N22A N 0.69443(6) 0.75426(14) 0.64523(9) 0.0199(5) Uani 1 1 d . . . C23A C 0.66910(8) 0.74002(18) 0.66916(11) 0.0212(6) Uani 1 1 d . . . C24A C 0.63456(8) 0.7651(2) 0.63385(12) 0.0303(7) Uani 1 1 d . . . H24A H 0.6122 0.7625 0.6413 0.036 Uiso 1 1 calc R . . C25A C 0.64002(8) 0.7943(2) 0.58628(12) 0.0291(7) Uani 1 1 d . . . H25A H 0.6219 0.8152 0.5537 0.035 Uiso 1 1 calc R . . C26A C 0.69496(8) 0.81025(18) 0.55508(11) 0.0226(6) Uani 1 1 d . . . H26A H 0.7156 0.8490 0.5739 0.027 Uiso 1 1 calc R . . H26B H 0.6781 0.8422 0.5232 0.027 Uiso 1 1 calc R . . N31A N 0.80563(7) 0.71046(16) 0.76893(10) 0.0246(5) Uani 1 1 d . . . C32A C 0.80858(9) 0.74983(19) 0.81700(12) 0.0289(7) Uani 1 1 d . . . H32A H 0.7877 0.7527 0.8284 0.035 Uiso 1 1 calc R . . C33A C 0.84057(9) 0.7866(2) 0.85110(12) 0.0317(7) Uani 1 1 d . . . H33A H 0.8416 0.8144 0.8849 0.038 Uiso 1 1 calc R . . C34A C 0.87090(9) 0.7818(2) 0.83454(13) 0.0373(8) Uani 1 1 d . . . H34A H 0.8933 0.8067 0.8568 0.045 Uiso 1 1 calc R . . C35A C 0.86831(9) 0.7404(2) 0.78523(13) 0.0342(8) Uani 1 1 d . . . H35A H 0.8889 0.7360 0.7733 0.041 Uiso 1 1 calc R . . C36A C 0.83528(8) 0.70524(19) 0.75342(12) 0.0242(6) Uani 1 1 d . . . N41A N 0.80225(7) 0.59893(15) 0.62243(10) 0.0222(5) Uani 1 1 d . . . N42A N 0.79826(6) 0.62855(15) 0.67030(9) 0.0207(5) Uani 1 1 d . . . C43A C 0.83039(8) 0.66378(18) 0.69920(12) 0.0230(6) Uani 1 1 d . . . C44A C 0.85472(8) 0.6564(2) 0.66947(13) 0.0321(7) Uani 1 1 d . . . H44A H 0.8791 0.6764 0.6805 0.039 Uiso 1 1 calc R . . C45A C 0.83591(8) 0.6140(2) 0.62097(13) 0.0306(7) Uani 1 1 d . . . H45A H 0.8450 0.5984 0.5919 0.037 Uiso 1 1 calc R . . C46A C 0.77157(8) 0.55754(18) 0.58077(12) 0.0240(6) Uani 1 1 d . . . H46A H 0.7588 0.5201 0.5999 0.029 Uiso 1 1 calc R . . H46B H 0.7809 0.5202 0.5568 0.029 Uiso 1 1 calc R . . C51A C 0.70884(8) 0.73288(17) 0.53389(11) 0.0201(6) Uani 1 1 d . . . C52A C 0.70042(8) 0.69378(18) 0.48425(11) 0.0232(6) Uani 1 1 d . . . H52A H 0.6822 0.7111 0.4507 0.028 Uiso 1 1 calc R . . C53A C 0.72427(8) 0.62054(19) 0.49145(12) 0.0239(6) Uani 1 1 d . . . H53A H 0.7250 0.5803 0.4636 0.029 Uiso 1 1 calc R . . C54A C 0.74525(8) 0.62030(18) 0.54513(11) 0.0214(6) Uani 1 1 d . . . O55A O 0.73675(5) 0.68937(12) 0.57266(7) 0.0215(4) Uani 1 1 d . . . N11B N 0.70549(6) 0.41890(15) 0.76474(9) 0.0206(5) Uani 1 1 d . . . C12B C 0.72102(8) 0.37606(19) 0.81266(11) 0.0245(6) Uani 1 1 d . . . H12B H 0.7455 0.3571 0.8212 0.029 Uiso 1 1 calc R . . C13B C 0.70307(9) 0.35834(19) 0.85011(12) 0.0261(6) Uani 1 1 d . . . H13B H 0.7146 0.3259 0.8829 0.031 Uiso 1 1 calc R . . C14B C 0.66795(9) 0.3889(2) 0.83872(13) 0.0305(7) Uani 1 1 d . . . H14B H 0.6552 0.3794 0.8643 0.037 Uiso 1 1 calc R . . C15B C 0.65175(8) 0.4334(2) 0.78979(13) 0.0278(7) Uani 1 1 d . . . H15B H 0.6277 0.4551 0.7811 0.033 Uiso 1 1 calc R . . C16B C 0.67119(8) 0.44619(18) 0.75328(12) 0.0228(6) Uani 1 1 d . . . N21B N 0.65064(6) 0.53681(15) 0.61844(10) 0.0234(5) Uani 1 1 d . . . N22B N 0.67449(6) 0.50363(15) 0.66592(9) 0.0212(5) Uani 1 1 d . . . C23B C 0.65434(8) 0.48806(18) 0.69863(12) 0.0223(6) Uani 1 1 d . . . C24B C 0.61809(8) 0.5119(2) 0.67243(13) 0.0284(7) Uani 1 1 d . . . H24B H 0.5986 0.5080 0.6870 0.034 Uiso 1 1 calc R . . C25B C 0.61688(8) 0.54223(19) 0.62119(13) 0.0286(7) Uani 1 1 d . . . H25B H 0.5960 0.5632 0.5928 0.034 Uiso 1 1 calc R . . C26B C 0.66303(9) 0.56093(19) 0.57191(12) 0.0278(7) Uani 1 1 d . . . H26C H 0.6849 0.5980 0.5861 0.033 Uiso 1 1 calc R . . H26D H 0.6438 0.5953 0.5448 0.033 Uiso 1 1 calc R . . N31B N 0.79546(7) 0.45889(15) 0.75398(9) 0.0224(5) Uani 1 1 d . . . C32B C 0.80750(9) 0.49019(19) 0.80630(12) 0.0266(6) Uani 1 1 d . . . H32B H 0.7901 0.5059 0.8234 0.032 Uiso 1 1 calc R . . C33B C 0.84397(9) 0.5007(2) 0.83642(13) 0.0305(7) Uani 1 1 d . . . H33B H 0.8514 0.5230 0.8733 0.037 Uiso 1 1 calc R . . C34B C 0.86937(9) 0.4780(2) 0.81166(13) 0.0345(8) Uani 1 1 d . . . H34B H 0.8946 0.4859 0.8309 0.041 Uiso 1 1 calc R . . C35B C 0.85748(9) 0.4437(2) 0.75842(13) 0.0301(7) Uani 1 1 d . . . H35B H 0.8745 0.4268 0.7409 0.036 Uiso 1 1 calc R . . C36B C 0.82032(8) 0.43434(18) 0.73082(12) 0.0221(6) Uani 1 1 d . . . N41B N 0.76801(7) 0.34041(15) 0.60245(9) 0.0242(5) Uani 1 1 d . . . N42B N 0.77159(7) 0.37265(15) 0.65347(9) 0.0223(5) Uani 1 1 d . . . C43B C 0.80649(8) 0.39639(18) 0.67477(11) 0.0229(6) Uani 1 1 d . . . C44B C 0.82533(9) 0.37767(19) 0.63741(12) 0.0265(7) Uani 1 1 d . . . H44B H 0.8503 0.3876 0.6426 0.032 Uiso 1 1 calc R . . C45B C 0.79988(9) 0.34228(19) 0.59222(12) 0.0268(7) Uani 1 1 d . . . H45B H 0.8038 0.3224 0.5593 0.032 Uiso 1 1 calc R . . C46B C 0.73334(9) 0.30540(19) 0.56733(12) 0.0278(7) Uani 1 1 d . . . H46C H 0.7235 0.2675 0.5903 0.033 Uiso 1 1 calc R . . H46D H 0.7376 0.2691 0.5380 0.033 Uiso 1 1 calc R . . C51B C 0.67197(8) 0.4853(2) 0.54277(12) 0.0256(6) Uani 1 1 d . . . C52B C 0.66035(9) 0.4563(2) 0.49023(13) 0.0334(8) Uani 1 1 d . . . H52B H 0.6411 0.4799 0.4601 0.040 Uiso 1 1 calc R . . C53B C 0.68217(9) 0.3835(2) 0.48800(13) 0.0333(8) Uani 1 1 d . . . H53B H 0.6806 0.3495 0.4562 0.040 Uiso 1 1 calc R . . C54B C 0.70547(8) 0.3724(2) 0.54002(12) 0.0263(6) Uani 1 1 d . . . O55B O 0.69976(6) 0.43410(12) 0.57500(8) 0.0250(5) Uani 1 1 d . . . N11C N 0.98062(7) 0.46483(16) 0.92584(10) 0.0263(6) Uani 1 1 d . . . C12C C 1.00270(8) 0.4157(2) 0.90715(13) 0.0303(7) Uani 1 1 d . . . H12C H 1.0159 0.4429 0.8862 0.036 Uiso 1 1 calc R . . C13C C 1.00723(9) 0.3280(2) 0.91672(13) 0.0327(7) Uani 1 1 d . . . H13C H 1.0232 0.2957 0.9030 0.039 Uiso 1 1 calc R . . C14C C 0.98794(9) 0.2886(2) 0.94680(13) 0.0329(7) Uani 1 1 d . . . H14C H 0.9901 0.2281 0.9534 0.040 Uiso 1 1 calc R . . C15C C 0.96559(9) 0.33741(19) 0.96714(12) 0.0280(7) Uani 1 1 d . . . H15C H 0.9525 0.3111 0.9886 0.034 Uiso 1 1 calc R . . C16C C 0.96228(8) 0.42551(19) 0.95602(11) 0.0218(6) Uani 1 1 d . . . N21C N 0.90930(6) 0.59240(16) 0.98481(10) 0.0237(5) Uani 1 1 d . . . N22C N 0.93048(7) 0.56047(15) 0.95657(10) 0.0238(5) Uani 1 1 d . . . C23C C 0.93864(8) 0.47994(19) 0.97642(11) 0.0220(6) Uani 1 1 d . . . C24C C 0.92188(8) 0.46081(19) 1.01621(12) 0.0243(6) Uani 1 1 d . . . H24C H 0.9231 0.4083 1.0361 0.029 Uiso 1 1 calc R . . C25C C 0.90337(8) 0.53416(19) 1.02010(12) 0.0250(6) Uani 1 1 d . . . H25C H 0.8890 0.5425 1.0435 0.030 Uiso 1 1 calc R . . C26C C 0.89181(8) 0.67707(19) 0.97063(13) 0.0279(7) Uani 1 1 d . . . H26E H 0.8768 0.6875 0.9948 0.033 Uiso 1 1 calc R . . H26F H 0.8751 0.6749 0.9317 0.033 Uiso 1 1 calc R . . N31C N 0.95389(7) 0.57374(18) 0.79559(11) 0.0307(6) Uani 1 1 d . . . C32C C 0.94948(9) 0.4975(2) 0.76891(14) 0.0372(8) Uani 1 1 d . . . H32C H 0.9482 0.4466 0.7892 0.045 Uiso 1 1 calc R . . C33C C 0.94669(9) 0.4891(3) 0.71361(15) 0.0413(9) Uani 1 1 d . . . H33C H 0.9433 0.4340 0.6961 0.050 Uiso 1 1 calc R . . C34C C 0.94891(9) 0.5628(3) 0.68434(15) 0.0427(9) Uani 1 1 d . . . H34C H 0.9469 0.5593 0.6461 0.051 Uiso 1 1 calc R . . C35C C 0.95402(8) 0.6415(2) 0.71113(13) 0.0338(8) Uani 1 1 d . . . H35C H 0.9560 0.6929 0.6918 0.041 Uiso 1 1 calc R . . C36C C 0.95630(8) 0.6449(2) 0.76706(12) 0.0270(7) Uani 1 1 d . . . N41C N 0.97379(7) 0.81283(17) 0.86733(10) 0.0274(6) Uani 1 1 d . . . N42C N 0.97107(7) 0.72816(16) 0.85331(10) 0.0261(5) Uani 1 1 d . . . C43C C 0.96223(8) 0.7271(2) 0.79720(12) 0.0259(6) Uani 1 1 d . . . C44C C 0.95971(9) 0.8112(2) 0.77651(13) 0.0329(7) Uani 1 1 d . . . H44C H 0.9540 0.8282 0.7387 0.040 Uiso 1 1 calc R . . C45C C 0.96706(9) 0.8640(2) 0.82169(14) 0.0331(7) Uani 1 1 d . . . H45C H 0.9674 0.9254 0.8213 0.040 Uiso 1 1 calc R . . C46C C 0.98543(9) 0.8391(2) 0.92575(13) 0.0314(7) Uani 1 1 d . . . H46E H 0.9931 0.9004 0.9285 0.038 Uiso 1 1 calc R . . H46F H 1.0068 0.8041 0.9469 0.038 Uiso 1 1 calc R . . C51C C 0.91673(8) 0.7517(2) 0.97620(12) 0.0256(6) Uani 1 1 d . . . C52C C 0.91832(10) 0.8294(2) 1.00007(14) 0.0339(7) Uani 1 1 d . . . H52C H 0.9049 0.8474 1.0233 0.041 Uiso 1 1 calc R . . C53C C 0.94384(10) 0.8800(2) 0.98418(14) 0.0353(8) Uani 1 1 d . . . H53C H 0.9505 0.9383 0.9944 0.042 Uiso 1 1 calc R . . C54C C 0.95672(9) 0.82886(19) 0.95166(12) 0.0282(7) Uani 1 1 d . . . O55C O 0.94017(5) 0.74905(13) 0.94606(8) 0.0245(4) Uani 1 1 d . . . Cl11 Cl 0.91493(2) 0.25806(5) 0.64708(3) 0.02901(16) Uani 1 1 d DU . . O12 O 0.90698(6) 0.28136(15) 0.69669(8) 0.0344(5) Uani 1 1 d DU A . O13X O 0.8918(8) 0.187(2) 0.6196(11) 0.035(4) Uani 0.47(13) 1 d PDU A 1 O14X O 0.9525(5) 0.231(2) 0.6625(8) 0.035(4) Uani 0.47(13) 1 d PDU A 1 O15X O 0.9088(11) 0.3312(15) 0.6104(10) 0.041(4) Uani 0.47(13) 1 d PDU A 1 O13Y O 0.8872(8) 0.201(3) 0.6132(12) 0.043(4) Uani 0.53(13) 1 d PDU A 2 O14Y O 0.9500(6) 0.216(3) 0.6622(8) 0.040(4) Uani 0.53(13) 1 d PDU A 2 O15Y O 0.9156(12) 0.3360(12) 0.6158(11) 0.036(4) Uani 0.53(13) 1 d PDU A 2 Cl21 Cl 0.90969(2) 0.79009(6) 0.57073(3) 0.0391(2) Uani 1 1 d DU . . O22 O 0.88647(8) 0.71687(16) 0.55554(12) 0.0571(7) Uani 1 1 d DU B . O23X O 0.90569(15) 0.8198(3) 0.6221(2) 0.0512(17) Uani 0.524(6) 1 d PDU B 1 O24X O 0.94469(12) 0.7422(3) 0.5871(2) 0.0435(15) Uani 0.524(6) 1 d PDU B 1 O25X O 0.9071(2) 0.8459(4) 0.5317(3) 0.061(2) Uani 0.524(6) 1 d PDU B 1 O23Y O 0.88530(13) 0.8658(3) 0.5744(3) 0.0479(18) Uani 0.476(6) 1 d PDU B 2 O24Y O 0.94213(14) 0.8005(4) 0.6151(2) 0.054(2) Uani 0.476(6) 1 d PDU B 2 O25Y O 0.9187(2) 0.8198(6) 0.5185(3) 0.061(2) Uani 0.476(6) 1 d PDU B 2 Cl31 Cl 0.78954(2) 0.56017(4) 0.94901(3) 0.02386(15) Uani 1 1 d DU . . O32 O 0.77016(7) 0.49996(14) 0.90621(8) 0.0396(6) Uani 1 1 d DU . . O33 O 0.76335(6) 0.60311(15) 0.96857(9) 0.0338(5) Uani 1 1 d DU . . O34 O 0.81530(6) 0.51417(15) 0.99411(9) 0.0361(5) Uani 1 1 d DU . . O35 O 0.80776(7) 0.62190(16) 0.92521(12) 0.0522(7) Uani 1 1 d DU . . C11S C 0.95965(12) 0.1850(3) 0.80565(17) 0.0570(11) Uani 1 1 d . . . H11A H 0.9819 0.1960 0.7966 0.086 Uiso 1 1 calc R . . H11B H 0.9510 0.2393 0.8167 0.086 Uiso 1 1 calc R . . H11C H 0.9409 0.1613 0.7729 0.086 Uiso 1 1 calc R . . C12S C 0.96744(10) 0.1230(2) 0.85149(17) 0.0420(9) Uani 1 1 d . . . N13S N 0.97316(9) 0.0738(2) 0.88666(14) 0.0485(8) Uani 1 1 d . . . C21S C 0.94377(12) 0.0177(3) 0.63128(17) 0.0503(10) Uani 1 1 d . . . H21A H 0.9208 0.0375 0.6043 0.076 Uiso 1 1 calc R . . H21B H 0.9495 -0.0402 0.6209 0.076 Uiso 1 1 calc R . . H21C H 0.9633 0.0577 0.6313 0.076 Uiso 1 1 calc R . . C22S C 0.94047(11) 0.0150(2) 0.68609(18) 0.0439(9) Uani 1 1 d . . . N23S N 0.93714(11) 0.0130(2) 0.72911(16) 0.0648(10) Uani 1 1 d . . . _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 0.01897(11) 0.03121(13) 0.02319(11) -0.00281(9) 0.00985(9) 0.00041(9) Ag2 0.02275(12) 0.03588(14) 0.02308(12) 0.00140(9) 0.01042(9) 0.00192(10) Ag3 0.03942(15) 0.02780(13) 0.02936(13) 0.00319(9) 0.01867(11) -0.00088(10) N11A 0.0216(12) 0.0223(12) 0.0211(11) -0.0018(9) 0.0088(10) 0.0011(10) C12A 0.0243(15) 0.0234(14) 0.0219(14) -0.0007(11) 0.0084(12) 0.0039(12) C13A 0.0343(17) 0.0240(15) 0.0213(14) -0.0001(12) 0.0118(13) -0.0010(13) C14A 0.0315(16) 0.0273(16) 0.0279(15) -0.0036(12) 0.0190(13) -0.0003(13) C15A 0.0247(15) 0.0264(16) 0.0281(15) -0.0015(12) 0.0120(12) 0.0058(13) C16A 0.0211(14) 0.0196(14) 0.0225(13) -0.0025(11) 0.0084(11) -0.0004(11) N21A 0.0252(12) 0.0214(12) 0.0168(11) -0.0003(9) 0.0068(10) 0.0033(10) N22A 0.0221(12) 0.0191(12) 0.0172(11) 0.0002(9) 0.0047(9) 0.0014(10) C23A 0.0218(14) 0.0208(14) 0.0219(13) -0.0050(11) 0.0082(11) 0.0014(12) C24A 0.0226(15) 0.0415(19) 0.0294(16) 0.0023(14) 0.0120(13) 0.0100(14) C25A 0.0262(16) 0.0342(18) 0.0248(15) 0.0005(13) 0.0054(12) 0.0112(14) C26A 0.0284(15) 0.0200(14) 0.0193(13) 0.0023(11) 0.0077(12) 0.0009(12) N31A 0.0240(13) 0.0251(13) 0.0251(12) 0.0006(10) 0.0085(10) 0.0012(11) C32A 0.0337(17) 0.0288(16) 0.0235(15) 0.0029(12) 0.0084(13) 0.0021(14) C33A 0.0413(19) 0.0262(16) 0.0217(15) 0.0024(12) 0.0022(13) 0.0005(14) C34A 0.0354(19) 0.0367(19) 0.0275(16) 0.0052(14) -0.0064(14) -0.0042(15) C35A 0.0209(15) 0.0425(19) 0.0353(17) 0.0080(15) 0.0039(13) 0.0012(14) C36A 0.0210(14) 0.0229(15) 0.0269(15) 0.0079(12) 0.0053(12) 0.0039(12) N41A 0.0248(13) 0.0221(12) 0.0234(12) 0.0021(10) 0.0131(10) 0.0059(10) N42A 0.0235(12) 0.0192(12) 0.0225(12) 0.0031(9) 0.0115(10) 0.0043(10) C43A 0.0193(14) 0.0230(15) 0.0272(15) 0.0050(12) 0.0085(12) 0.0056(12) C44A 0.0183(15) 0.0414(19) 0.0380(18) 0.0035(15) 0.0110(13) 0.0028(14) C45A 0.0268(16) 0.0367(18) 0.0350(17) 0.0046(14) 0.0195(14) 0.0093(14) C46A 0.0295(16) 0.0208(15) 0.0239(14) 0.0006(11) 0.0119(12) 0.0011(12) C51A 0.0221(14) 0.0177(13) 0.0205(13) 0.0047(11) 0.0073(11) -0.0016(11) C52A 0.0275(15) 0.0226(14) 0.0210(13) 0.0023(11) 0.0099(12) -0.0021(12) C53A 0.0282(15) 0.0237(15) 0.0233(14) -0.0016(12) 0.0132(12) -0.0025(13) C54A 0.0278(15) 0.0169(14) 0.0220(14) 0.0007(11) 0.0114(12) -0.0027(12) O55A 0.0291(11) 0.0168(9) 0.0191(9) 0.0006(7) 0.0086(8) 0.0032(8) N11B 0.0226(12) 0.0211(12) 0.0188(11) -0.0014(9) 0.0077(10) -0.0013(10) C12B 0.0275(15) 0.0258(15) 0.0205(14) -0.0014(12) 0.0081(12) -0.0001(13) C13B 0.0337(17) 0.0274(15) 0.0176(13) -0.0005(12) 0.0088(12) -0.0027(13) C14B 0.0343(17) 0.0373(18) 0.0252(15) -0.0035(13) 0.0170(13) -0.0034(15) C15B 0.0252(15) 0.0325(17) 0.0299(16) -0.0024(13) 0.0148(13) -0.0010(13) C16B 0.0271(15) 0.0194(14) 0.0222(14) -0.0066(11) 0.0088(12) -0.0028(12) N21B 0.0232(12) 0.0229(12) 0.0226(12) 0.0037(10) 0.0056(10) 0.0016(10) N22B 0.0218(12) 0.0187(12) 0.0212(12) 0.0004(9) 0.0048(10) -0.0006(10) C23B 0.0246(14) 0.0170(14) 0.0264(14) -0.0032(11) 0.0100(12) -0.0013(12) C24B 0.0231(15) 0.0289(16) 0.0339(16) 0.0008(13) 0.0105(13) 0.0014(13) C25B 0.0243(15) 0.0275(16) 0.0305(16) 0.0016(13) 0.0045(13) 0.0029(13) C26B 0.0283(16) 0.0283(16) 0.0259(15) 0.0089(12) 0.0078(13) -0.0029(13) N31B 0.0254(13) 0.0237(12) 0.0202(12) 0.0023(9) 0.0103(10) 0.0042(10) C32B 0.0331(16) 0.0265(16) 0.0234(14) 0.0008(12) 0.0137(13) 0.0061(13) C33B 0.0330(17) 0.0322(17) 0.0250(15) -0.0030(13) 0.0078(13) 0.0019(14) C34B 0.0262(16) 0.047(2) 0.0293(16) 0.0010(15) 0.0075(13) 0.0001(15) C35B 0.0275(16) 0.0389(19) 0.0267(16) 0.0038(13) 0.0125(13) 0.0066(14) C36B 0.0263(15) 0.0197(14) 0.0228(14) 0.0062(11) 0.0114(12) 0.0052(12) N41B 0.0346(14) 0.0206(12) 0.0209(12) 0.0012(10) 0.0138(11) 0.0037(11) N42B 0.0330(14) 0.0194(12) 0.0174(11) 0.0017(9) 0.0123(10) 0.0031(11) C43B 0.0275(15) 0.0234(15) 0.0202(14) 0.0065(11) 0.0112(12) 0.0090(12) C44B 0.0311(16) 0.0286(16) 0.0242(15) 0.0051(12) 0.0151(13) 0.0093(13) C45B 0.0357(17) 0.0239(15) 0.0251(15) 0.0070(12) 0.0161(13) 0.0105(13) C46B 0.0390(18) 0.0224(15) 0.0260(15) -0.0046(12) 0.0162(13) -0.0051(14) C51B 0.0225(15) 0.0287(16) 0.0235(14) 0.0047(12) 0.0045(12) -0.0063(13) C52B 0.0237(16) 0.053(2) 0.0216(15) 0.0015(14) 0.0047(12) -0.0085(15) C53B 0.0333(17) 0.046(2) 0.0219(15) -0.0085(14) 0.0102(13) -0.0097(16) C54B 0.0292(16) 0.0286(16) 0.0247(15) -0.0054(12) 0.0139(13) -0.0098(13) O55B 0.0338(12) 0.0214(10) 0.0181(10) -0.0024(8) 0.0062(9) -0.0019(9) N11C 0.0270(13) 0.0289(14) 0.0259(13) -0.0039(10) 0.0126(11) -0.0024(11) C12C 0.0246(16) 0.0391(18) 0.0304(16) -0.0061(14) 0.0133(13) -0.0019(14) C13C 0.0260(16) 0.0419(19) 0.0295(16) -0.0066(14) 0.0085(13) 0.0094(15) C14C 0.0391(19) 0.0289(17) 0.0298(16) 0.0019(13) 0.0100(14) 0.0092(15) C15C 0.0312(16) 0.0302(16) 0.0236(14) 0.0016(12) 0.0104(13) 0.0037(14) C16C 0.0212(14) 0.0256(14) 0.0176(13) -0.0006(11) 0.0052(11) -0.0012(12) N21C 0.0210(12) 0.0273(13) 0.0259(12) 0.0013(10) 0.0118(10) 0.0040(10) N22C 0.0222(12) 0.0273(13) 0.0247(12) 0.0013(10) 0.0114(10) 0.0033(11) C23C 0.0225(14) 0.0250(15) 0.0188(13) -0.0004(11) 0.0071(11) -0.0027(12) C24C 0.0290(16) 0.0228(15) 0.0221(14) -0.0002(11) 0.0098(12) -0.0047(13) C25C 0.0259(15) 0.0300(16) 0.0222(14) -0.0016(12) 0.0120(12) -0.0052(13) C26C 0.0246(15) 0.0299(16) 0.0319(16) 0.0049(13) 0.0131(13) 0.0076(13) N31C 0.0261(13) 0.0376(15) 0.0312(14) -0.0049(12) 0.0135(11) -0.0060(12) C32C 0.0338(18) 0.0393(19) 0.0432(19) -0.0080(16) 0.0191(15) -0.0061(16) C33C 0.0307(18) 0.053(2) 0.042(2) -0.0151(18) 0.0141(16) 0.0002(17) C34C 0.0258(17) 0.071(3) 0.0316(18) -0.0107(18) 0.0091(14) 0.0079(18) C35C 0.0227(16) 0.053(2) 0.0269(16) 0.0010(15) 0.0103(13) 0.0072(15) C36C 0.0162(14) 0.0386(18) 0.0262(15) 0.0003(13) 0.0073(12) 0.0002(13) N41C 0.0278(14) 0.0271(13) 0.0279(13) 0.0032(11) 0.0101(11) -0.0021(11) N42C 0.0246(13) 0.0292(14) 0.0262(13) 0.0013(11) 0.0106(10) 0.0001(11) C43C 0.0191(14) 0.0381(18) 0.0226(14) 0.0055(13) 0.0097(12) 0.0032(13) C44C 0.0309(17) 0.0410(19) 0.0286(16) 0.0101(14) 0.0120(14) 0.0020(15) C45C 0.0281(17) 0.0330(17) 0.0403(18) 0.0120(15) 0.0144(14) 0.0014(14) C46C 0.0303(17) 0.0326(17) 0.0302(16) -0.0023(13) 0.0084(14) -0.0031(14) C51C 0.0237(15) 0.0312(16) 0.0239(14) 0.0067(12) 0.0106(12) 0.0084(13) C52C 0.0397(19) 0.0297(17) 0.0364(18) 0.0008(14) 0.0181(15) 0.0077(15) C53C 0.044(2) 0.0255(16) 0.0368(18) -0.0017(14) 0.0143(16) 0.0061(15) C54C 0.0281(16) 0.0262(16) 0.0284(15) 0.0012(13) 0.0068(13) 0.0005(13) O55C 0.0249(11) 0.0250(11) 0.0249(10) -0.0012(8) 0.0100(8) 0.0012(9) Cl11 0.0287(4) 0.0314(4) 0.0316(4) 0.0037(3) 0.0163(3) 0.0007(3) O12 0.0357(13) 0.0439(14) 0.0286(11) 0.0020(10) 0.0172(10) 0.0016(11) O13X 0.032(6) 0.038(6) 0.042(5) -0.005(5) 0.021(5) -0.008(5) O14X 0.024(4) 0.033(8) 0.051(6) 0.018(5) 0.017(4) 0.001(4) O15X 0.043(9) 0.043(6) 0.039(6) 0.013(4) 0.016(5) 0.007(5) O13Y 0.036(6) 0.055(8) 0.042(5) -0.017(6) 0.017(4) -0.010(6) O14Y 0.031(5) 0.030(8) 0.066(6) 0.009(4) 0.027(4) 0.004(4) O15Y 0.045(9) 0.037(5) 0.030(5) 0.014(3) 0.018(5) 0.004(4) Cl21 0.0256(4) 0.0591(6) 0.0325(4) -0.0136(4) 0.0093(3) 0.0040(4) O22 0.072(2) 0.0355(14) 0.0727(19) -0.0134(13) 0.0356(16) -0.0056(14) O23X 0.067(4) 0.048(3) 0.052(3) -0.027(3) 0.038(3) -0.012(3) O24X 0.027(2) 0.055(3) 0.051(3) 0.008(3) 0.017(2) 0.006(2) O25X 0.088(6) 0.044(4) 0.038(4) 0.013(3) 0.004(3) 0.002(3) O23Y 0.032(3) 0.032(3) 0.086(5) -0.015(3) 0.028(3) 0.003(2) O24Y 0.034(3) 0.062(4) 0.051(4) 0.017(3) -0.004(3) 0.002(3) O25Y 0.061(5) 0.085(6) 0.044(4) -0.008(4) 0.029(3) -0.012(4) Cl31 0.0289(4) 0.0192(3) 0.0281(4) -0.0005(3) 0.0157(3) -0.0010(3) O32 0.0614(16) 0.0275(12) 0.0246(11) -0.0050(9) 0.0069(11) 0.0041(12) O33 0.0307(12) 0.0446(14) 0.0303(12) -0.0066(10) 0.0158(10) 0.0072(10) O34 0.0327(12) 0.0392(13) 0.0329(12) -0.0025(10) 0.0061(10) 0.0037(11) O35 0.0490(16) 0.0332(14) 0.091(2) 0.0156(14) 0.0459(15) -0.0008(12) C11S 0.054(3) 0.053(2) 0.052(2) 0.000(2) 0.001(2) -0.004(2) C12S 0.0284(18) 0.040(2) 0.053(2) -0.0079(18) 0.0062(16) -0.0055(16) N13S 0.0436(19) 0.0430(18) 0.055(2) -0.0054(16) 0.0105(16) -0.0075(16) C21S 0.055(2) 0.041(2) 0.059(2) -0.0025(19) 0.024(2) 0.0006(19) C22S 0.046(2) 0.0303(19) 0.056(2) 0.0052(17) 0.0172(19) -0.0015(17) N23S 0.087(3) 0.048(2) 0.062(2) 0.0095(18) 0.028(2) -0.006(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. ; _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 N42A 2.231(2) . ? Ag1 N11A 2.236(2) . ? Ag1 N31A 2.479(2) . ? Ag1 N22A 2.575(2) . ? Ag1 Ag2 3.2932(3) . ? Ag2 N22B 2.343(2) . ? Ag2 N31B 2.344(2) . ? Ag2 N11B 2.369(2) . ? Ag2 N42B 2.438(2) . ? Ag3 N42C 2.263(3) . ? Ag3 N11C 2.319(3) . ? Ag3 N22C 2.402(2) . ? Ag3 N31C 2.512(3) . ? N11A C12A 1.347(3) . ? N11A C16A 1.348(4) . ? C12A C13A 1.377(4) . ? C12A H12A 0.9500 . ? C13A C14A 1.385(4) . ? C13A H13A 0.9500 . ? C14A C15A 1.384(4) . ? C14A H14A 0.9500 . ? C15A C16A 1.391(4) . ? C15A H15A 0.9500 . ? C16A C23A 1.469(4) . ? N21A C25A 1.345(4) . ? N21A N22A 1.356(3) . ? N21A C26A 1.473(4) . ? N22A C23A 1.337(4) . ? C23A C24A 1.403(4) . ? C24A C25A 1.371(4) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C26A C51A 1.485(4) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? N31A C32A 1.336(4) . ? N31A C36A 1.339(4) . ? C32A C33A 1.384(4) . ? C32A H32A 0.9500 . ? C33A C34A 1.380(5) . ? C33A H33A 0.9500 . ? C34A C35A 1.382(5) . ? C34A H34A 0.9500 . ? C35A C36A 1.385(4) . ? C35A H35A 0.9500 . ? C36A C43A 1.474(4) . ? N41A C45A 1.343(4) . ? N41A N42A 1.356(3) . ? N41A C46A 1.458(4) . ? N42A C43A 1.340(4) . ? C43A C44A 1.398(4) . ? C44A C45A 1.375(5) . ? C44A H44A 0.9500 . ? C45A H45A 0.9500 . ? C46A C54A 1.484(4) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C51A C52A 1.339(4) . ? C51A O55A 1.378(3) . ? C52A C53A 1.438(4) . ? C52A H52A 0.9500 . ? C53A C54A 1.339(4) . ? C53A H53A 0.9500 . ? C54A O55A 1.376(3) . ? N11B C16B 1.338(4) . ? N11B C12B 1.343(4) . ? C12B C13B 1.381(4) . ? C12B H12B 0.9500 . ? C13B C14B 1.384(4) . ? C13B H13B 0.9500 . ? C14B C15B 1.379(4) . ? C14B H14B 0.9500 . ? C15B C16B 1.391(4) . ? C15B H15B 0.9500 . ? C16B C23B 1.476(4) . ? N21B C25B 1.342(4) . ? N21B N22B 1.358(3) . ? N21B C26B 1.465(4) . ? N22B C23B 1.340(4) . ? C23B C24B 1.397(4) . ? C24B C25B 1.370(4) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B C51B 1.486(4) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? N31B C36B 1.343(4) . ? N31B C32B 1.346(4) . ? C32B C33B 1.383(4) . ? C32B H32B 0.9500 . ? C33B C34B 1.381(5) . ? C33B H33B 0.9500 . ? C34B C35B 1.383(4) . ? C34B H34B 0.9500 . ? C35B C36B 1.392(4) . ? C35B H35B 0.9500 . ? C36B C43B 1.469(4) . ? N41B C45B 1.349(4) . ? N41B N42B 1.353(3) . ? N41B C46B 1.455(4) . ? N42B C43B 1.338(4) . ? C43B C44B 1.408(4) . ? C44B C45B 1.360(4) . ? C44B H44B 0.9500 . ? C45B H45B 0.9500 . ? C46B C54B 1.496(4) . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C51B C52B 1.338(4) . ? C51B O55B 1.373(3) . ? C52B C53B 1.423(5) . ? C52B H52B 0.9500 . ? C53B C54B 1.345(4) . ? C53B H53B 0.9500 . ? C54B O55B 1.372(4) . ? N11C C12C 1.346(4) . ? N11C C16C 1.352(4) . ? C12C C13C 1.378(5) . ? C12C H12C 0.9500 . ? C13C C14C 1.378(5) . ? C13C H13C 0.9500 . ? C14C C15C 1.375(4) . ? C14C H14C 0.9500 . ? C15C C16C 1.389(4) . ? C15C H15C 0.9500 . ? C16C C23C 1.462(4) . ? N21C C25C 1.344(4) . ? N21C N22C 1.352(3) . ? N21C C26C 1.465(4) . ? N22C C23C 1.342(4) . ? C23C C24C 1.404(4) . ? C24C C25C 1.365(4) . ? C24C H24C 0.9500 . ? C25C H25C 0.9500 . ? C26C C51C 1.484(4) . ? C26C H26E 0.9900 . ? C26C H26F 0.9900 . ? N31C C36C 1.338(4) . ? N31C C32C 1.343(4) . ? C32C C33C 1.380(5) . ? C32C H32C 0.9500 . ? C33C C34C 1.381(5) . ? C33C H33C 0.9500 . ? C34C C35C 1.377(5) . ? C34C H34C 0.9500 . ? C35C C36C 1.396(4) . ? C35C H35C 0.9500 . ? C36C C43C 1.463(4) . ? N41C N42C 1.352(4) . ? N41C C45C 1.357(4) . ? N41C C46C 1.460(4) . ? N42C C43C 1.352(4) . ? C43C C44C 1.395(4) . ? C44C C45C 1.360(5) . ? C44C H44C 0.9500 . ? C45C H45C 0.9500 . ? C46C C54C 1.481(5) . ? C46C H46E 0.9900 . ? C46C H46F 0.9900 . ? C51C C52C 1.338(4) . ? C51C O55C 1.372(4) . ? C52C C53C 1.424(5) . ? C52C H52C 0.9500 . ? C53C C54C 1.354(5) . ? C53C H53C 0.9500 . ? C54C O55C 1.378(4) . ? Cl11 O15X 1.436(14) . ? Cl11 O13Y 1.438(13) . ? Cl11 O12 1.439(2) . ? Cl11 O14Y 1.443(13) . ? Cl11 O13X 1.444(14) . ? Cl11 O14X 1.449(13) . ? Cl11 O15Y 1.450(13) . ? Cl21 O25X 1.294(6) . ? Cl21 O24Y 1.399(5) . ? Cl21 O22 1.421(3) . ? Cl21 O23X 1.441(4) . ? Cl21 O24X 1.485(4) . ? Cl21 O23Y 1.530(5) . ? Cl21 O25Y 1.551(7) . ? Cl31 O33 1.436(2) . ? Cl31 O35 1.437(2) . ? Cl31 O34 1.438(2) . ? Cl31 O32 1.442(2) . ? C11S C12S 1.461(6) . ? C11S H11A 0.9800 . ? C11S H11B 0.9800 . ? C11S H11C 0.9800 . ? C12S N13S 1.139(5) . ? C21S C22S 1.441(6) . ? C21S H21A 0.9800 . ? C21S H21B 0.9800 . ? C21S H21C 0.9800 . ? C22S N23S 1.143(5) . ? _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 N42A Ag1 N11A 160.89(8) . . ? N42A Ag1 N31A 70.87(8) . . ? N11A Ag1 N31A 97.33(8) . . ? N42A Ag1 N22A 128.98(8) . . ? N11A Ag1 N22A 70.05(8) . . ? N31A Ag1 N22A 125.14(8) . . ? N42A Ag1 Ag2 88.58(6) . . ? N11A Ag1 Ag2 82.80(6) . . ? N31A Ag1 Ag2 114.81(6) . . ? N22A Ag1 Ag2 115.94(5) . . ? N22B Ag2 N31B 152.46(8) . . ? N22B Ag2 N11B 71.00(8) . . ? N31B Ag2 N11B 101.71(8) . . ? N22B Ag2 N42B 133.39(8) . . ? N31B Ag2 N42B 70.39(8) . . ? N11B Ag2 N42B 136.45(8) . . ? N22B Ag2 Ag1 79.58(6) . . ? N31B Ag2 Ag1 78.44(6) . . ? N11B Ag2 Ag1 110.60(6) . . ? N42B Ag2 Ag1 109.43(6) . . ? N42C Ag3 N11C 150.96(9) . . ? N42C Ag3 N22C 137.00(9) . . ? N11C Ag3 N22C 71.51(8) . . ? N42C Ag3 N31C 70.61(9) . . ? N11C Ag3 N31C 94.53(9) . . ? N22C Ag3 N31C 131.43(8) . . ? C12A N11A C16A 118.2(2) . . ? C12A N11A Ag1 120.29(19) . . ? C16A N11A Ag1 121.48(18) . . ? N11A C12A C13A 123.3(3) . . ? N11A C12A H12A 118.3 . . ? C13A C12A H12A 118.3 . . ? C12A C13A C14A 118.4(3) . . ? C12A C13A H13A 120.8 . . ? C14A C13A H13A 120.8 . . ? C15A C14A C13A 119.1(3) . . ? C15A C14A H14A 120.5 . . ? C13A C14A H14A 120.5 . . ? C14A C15A C16A 119.5(3) . . ? C14A C15A H15A 120.2 . . ? C16A C15A H15A 120.2 . . ? N11A C16A C15A 121.4(3) . . ? N11A C16A C23A 117.2(2) . . ? C15A C16A C23A 121.4(3) . . ? C25A N21A N22A 112.2(2) . . ? C25A N21A C26A 127.4(2) . . ? N22A N21A C26A 120.4(2) . . ? C23A N22A N21A 104.7(2) . . ? C23A N22A Ag1 107.73(17) . . ? N21A N22A Ag1 141.82(18) . . ? N22A C23A C24A 111.0(2) . . ? N22A C23A C16A 120.2(2) . . ? C24A C23A C16A 128.8(3) . . ? C25A C24A C23A 105.1(3) . . ? C25A C24A H24A 127.4 . . ? C23A C24A H24A 127.4 . . ? N21A C25A C24A 107.0(3) . . ? N21A C25A H25A 126.5 . . ? C24A C25A H25A 126.5 . . ? N21A C26A C51A 112.3(2) . . ? N21A C26A H26A 109.1 . . ? C51A C26A H26A 109.1 . . ? N21A C26A H26B 109.1 . . ? C51A C26A H26B 109.1 . . ? H26A C26A H26B 107.9 . . ? C32A N31A C36A 118.3(3) . . ? C32A N31A Ag1 128.6(2) . . ? C36A N31A Ag1 112.62(18) . . ? N31A C32A C33A 123.3(3) . . ? N31A C32A H32A 118.4 . . ? C33A C32A H32A 118.4 . . ? C34A C33A C32A 118.1(3) . . ? C34A C33A H33A 121.0 . . ? C32A C33A H33A 121.0 . . ? C33A C34A C35A 119.2(3) . . ? C33A C34A H34A 120.4 . . ? C35A C34A H34A 120.4 . . ? C34A C35A C36A 119.2(3) . . ? C34A C35A H35A 120.4 . . ? C36A C35A H35A 120.4 . . ? N31A C36A C35A 121.9(3) . . ? N31A C36A C43A 116.3(3) . . ? C35A C36A C43A 121.7(3) . . ? C45A N41A N42A 111.5(2) . . ? C45A N41A C46A 129.0(3) . . ? N42A N41A C46A 119.4(2) . . ? C43A N42A N41A 105.5(2) . . ? C43A N42A Ag1 118.62(19) . . ? N41A N42A Ag1 133.38(18) . . ? N42A C43A C44A 110.3(3) . . ? N42A C43A C36A 119.9(3) . . ? C44A C43A C36A 129.7(3) . . ? C45A C44A C43A 105.5(3) . . ? C45A C44A H44A 127.2 . . ? C43A C44A H44A 127.2 . . ? N41A C45A C44A 107.1(3) . . ? N41A C45A H45A 126.4 . . ? C44A C45A H45A 126.4 . . ? N41A C46A C54A 113.1(2) . . ? N41A C46A H46A 109.0 . . ? C54A C46A H46A 109.0 . . ? N41A C46A H46B 109.0 . . ? C54A C46A H46B 109.0 . . ? H46A C46A H46B 107.8 . . ? C52A C51A O55A 110.1(2) . . ? C52A C51A C26A 134.5(3) . . ? O55A C51A C26A 115.4(2) . . ? C51A C52A C53A 106.8(3) . . ? C51A C52A H52A 126.6 . . ? C53A C52A H52A 126.6 . . ? C54A C53A C52A 106.4(3) . . ? C54A C53A H53A 126.8 . . ? C52A C53A H53A 126.8 . . ? C53A C54A O55A 110.4(2) . . ? C53A C54A C46A 133.7(3) . . ? O55A C54A C46A 115.5(2) . . ? C54A O55A C51A 106.3(2) . . ? C16B N11B C12B 118.2(3) . . ? C16B N11B Ag2 116.81(18) . . ? C12B N11B Ag2 125.0(2) . . ? N11B C12B C13B 123.0(3) . . ? N11B C12B H12B 118.5 . . ? C13B C12B H12B 118.5 . . ? C12B C13B C14B 118.5(3) . . ? C12B C13B H13B 120.8 . . ? C14B C13B H13B 120.8 . . ? C15B C14B C13B 119.1(3) . . ? C15B C14B H14B 120.5 . . ? C13B C14B H14B 120.5 . . ? C14B C15B C16B 119.0(3) . . ? C14B C15B H15B 120.5 . . ? C16B C15B H15B 120.5 . . ? N11B C16B C15B 122.2(3) . . ? N11B C16B C23B 116.5(3) . . ? C15B C16B C23B 121.3(3) . . ? C25B N21B N22B 111.8(2) . . ? C25B N21B C26B 127.9(2) . . ? N22B N21B C26B 120.2(2) . . ? C23B N22B N21B 104.5(2) . . ? C23B N22B Ag2 115.92(18) . . ? N21B N22B Ag2 138.71(19) . . ? N22B C23B C24B 111.3(3) . . ? N22B C23B C16B 119.6(3) . . ? C24B C23B C16B 129.1(3) . . ? C25B C24B C23B 104.9(3) . . ? C25B C24B H24B 127.6 . . ? C23B C24B H24B 127.6 . . ? N21B C25B C24B 107.5(3) . . ? N21B C25B H25B 126.2 . . ? C24B C25B H25B 126.2 . . ? N21B C26B C51B 113.3(2) . . ? N21B C26B H26C 108.9 . . ? C51B C26B H26C 108.9 . . ? N21B C26B H26D 108.9 . . ? C51B C26B H26D 108.9 . . ? H26C C26B H26D 107.7 . . ? C36B N31B C32B 117.9(3) . . ? C36B N31B Ag2 117.08(18) . . ? C32B N31B Ag2 124.9(2) . . ? N31B C32B C33B 123.3(3) . . ? N31B C32B H32B 118.4 . . ? C33B C32B H32B 118.4 . . ? C34B C33B C32B 118.5(3) . . ? C34B C33B H33B 120.8 . . ? C32B C33B H33B 120.8 . . ? C33B C34B C35B 118.9(3) . . ? C33B C34B H34B 120.5 . . ? C35B C34B H34B 120.5 . . ? C34B C35B C36B 119.4(3) . . ? C34B C35B H35B 120.3 . . ? C36B C35B H35B 120.3 . . ? N31B C36B C35B 121.9(3) . . ? N31B C36B C43B 116.8(3) . . ? C35B C36B C43B 121.2(3) . . ? C45B N41B N42B 111.5(2) . . ? C45B N41B C46B 128.0(2) . . ? N42B N41B C46B 120.5(2) . . ? C43B N42B N41B 105.0(2) . . ? C43B N42B Ag2 111.03(18) . . ? N41B N42B Ag2 137.63(19) . . ? N42B C43B C44B 110.9(3) . . ? N42B C43B C36B 120.1(3) . . ? C44B C43B C36B 129.0(3) . . ? C45B C44B C43B 104.8(3) . . ? C45B C44B H44B 127.6 . . ? C43B C44B H44B 127.6 . . ? N41B C45B C44B 107.8(3) . . ? N41B C45B H45B 126.1 . . ? C44B C45B H45B 126.1 . . ? N41B C46B C54B 114.3(2) . . ? N41B C46B H46C 108.7 . . ? C54B C46B H46C 108.7 . . ? N41B C46B H46D 108.7 . . ? C54B C46B H46D 108.7 . . ? H46C C46B H46D 107.6 . . ? C52B C51B O55B 110.0(3) . . ? C52B C51B C26B 134.7(3) . . ? O55B C51B C26B 115.1(2) . . ? C51B C52B C53B 107.2(3) . . ? C51B C52B H52B 126.4 . . ? C53B C52B H52B 126.4 . . ? C54B C53B C52B 106.2(3) . . ? C54B C53B H53B 126.9 . . ? C52B C53B H53B 126.9 . . ? C53B C54B O55B 110.3(3) . . ? C53B C54B C46B 134.1(3) . . ? O55B C54B C46B 115.4(2) . . ? C54B O55B C51B 106.2(2) . . ? C12C N11C C16C 117.6(3) . . ? C12C N11C Ag3 124.3(2) . . ? C16C N11C Ag3 117.07(19) . . ? N11C C12C C13C 123.6(3) . . ? N11C C12C H12C 118.2 . . ? C13C C12C H12C 118.2 . . ? C12C C13C C14C 118.2(3) . . ? C12C C13C H13C 120.9 . . ? C14C C13C H13C 120.9 . . ? C15C C14C C13C 119.6(3) . . ? C15C C14C H14C 120.2 . . ? C13C C14C H14C 120.2 . . ? C14C C15C C16C 119.4(3) . . ? C14C C15C H15C 120.3 . . ? C16C C15C H15C 120.3 . . ? N11C C16C C15C 121.7(3) . . ? N11C C16C C23C 117.0(3) . . ? C15C C16C C23C 121.3(3) . . ? C25C N21C N22C 112.2(2) . . ? C25C N21C C26C 126.6(3) . . ? N22C N21C C26C 120.7(2) . . ? C23C N22C N21C 104.5(2) . . ? C23C N22C Ag3 113.28(19) . . ? N21C N22C Ag3 141.40(18) . . ? N22C C23C C24C 110.9(3) . . ? N22C C23C C16C 120.0(3) . . ? C24C C23C C16C 129.1(3) . . ? C25C C24C C23C 105.0(3) . . ? C25C C24C H24C 127.5 . . ? C23C C24C H24C 127.5 . . ? N21C C25C C24C 107.3(3) . . ? N21C C25C H25C 126.3 . . ? C24C C25C H25C 126.3 . . ? N21C C26C C51C 115.8(2) . . ? N21C C26C H26E 108.3 . . ? C51C C26C H26E 108.3 . . ? N21C C26C H26F 108.3 . . ? C51C C26C H26F 108.3 . . ? H26E C26C H26F 107.4 . . ? C36C N31C C32C 118.0(3) . . ? C36C N31C Ag3 112.4(2) . . ? C32C N31C Ag3 129.5(2) . . ? N31C C32C C33C 123.4(3) . . ? N31C C32C H32C 118.3 . . ? C33C C32C H32C 118.3 . . ? C32C C33C C34C 118.2(3) . . ? C32C C33C H33C 120.9 . . ? C34C C33C H33C 120.9 . . ? C35C C34C C33C 119.3(3) . . ? C35C C34C H34C 120.4 . . ? C33C C34C H34C 120.4 . . ? C34C C35C C36C 119.1(3) . . ? C34C C35C H35C 120.4 . . ? C36C C35C H35C 120.4 . . ? N31C C36C C35C 122.0(3) . . ? N31C C36C C43C 117.3(3) . . ? C35C C36C C43C 120.7(3) . . ? N42C N41C C45C 111.3(3) . . ? N42C N41C C46C 120.5(2) . . ? C45C N41C C46C 128.0(3) . . ? N41C N42C C43C 105.1(2) . . ? N41C N42C Ag3 134.30(19) . . ? C43C N42C Ag3 118.2(2) . . ? N42C C43C C44C 110.3(3) . . ? N42C C43C C36C 120.3(3) . . ? C44C C43C C36C 129.4(3) . . ? C45C C44C C43C 105.8(3) . . ? C45C C44C H44C 127.1 . . ? C43C C44C H44C 127.1 . . ? N41C C45C C44C 107.4(3) . . ? N41C C45C H45C 126.3 . . ? C44C C45C H45C 126.3 . . ? N41C C46C C54C 113.3(3) . . ? N41C C46C H46E 108.9 . . ? C54C C46C H46E 108.9 . . ? N41C C46C H46F 108.9 . . ? C54C C46C H46F 108.9 . . ? H46E C46C H46F 107.7 . . ? C52C C51C O55C 109.9(3) . . ? C52C C51C C26C 132.3(3) . . ? O55C C51C C26C 117.2(3) . . ? C51C C52C C53C 107.3(3) . . ? C51C C52C H52C 126.3 . . ? C53C C52C H52C 126.3 . . ? C54C C53C C52C 106.6(3) . . ? C54C C53C H53C 126.7 . . ? C52C C53C H53C 126.7 . . ? C53C C54C O55C 109.4(3) . . ? C53C C54C C46C 134.0(3) . . ? O55C C54C C46C 116.4(3) . . ? C51C O55C C54C 106.9(2) . . ? O15X Cl11 O13Y 99.4(19) . . ? O15X Cl11 O12 109.6(9) . . ? O13Y Cl11 O12 110.0(8) . . ? O15X Cl11 O14Y 117.7(19) . . ? O13Y Cl11 O14Y 110.1(8) . . ? O12 Cl11 O14Y 109.6(8) . . ? O15X Cl11 O13X 109.9(9) . . ? O13Y Cl11 O13X 12(2) . . ? O12 Cl11 O13X 109.5(8) . . ? O14Y Cl11 O13X 100.1(19) . . ? O15X Cl11 O14X 109.9(9) . . ? O13Y Cl11 O14X 118.4(18) . . ? O12 Cl11 O14X 109.0(8) . . ? O14Y Cl11 O14X 10(2) . . ? O13X Cl11 O14X 108.9(9) . . ? O15X Cl11 O15Y 11(2) . . ? O13Y Cl11 O15Y 109.1(8) . . ? O12 Cl11 O15Y 108.7(8) . . ? O14Y Cl11 O15Y 109.3(8) . . ? O13X Cl11 O15Y 119.1(17) . . ? O14X Cl11 O15Y 101.0(19) . . ? O25X Cl21 O24Y 111.3(4) . . ? O25X Cl21 O22 116.2(3) . . ? O24Y Cl21 O22 129.5(3) . . ? O25X Cl21 O23X 118.7(4) . . ? O24Y Cl21 O23X 64.5(3) . . ? O22 Cl21 O23X 104.5(2) . . ? O25X Cl21 O24X 112.3(4) . . ? O24Y Cl21 O24X 47.9(3) . . ? O22 Cl21 O24X 97.0(2) . . ? O23X Cl21 O24X 105.5(3) . . ? O25X Cl21 O23Y 69.1(4) . . ? O24Y Cl21 O23Y 106.0(3) . . ? O22 Cl21 O23Y 106.0(2) . . ? O23X Cl21 O23Y 56.4(3) . . ? O24X Cl21 O23Y 153.6(3) . . ? O25X Cl21 O25Y 29.2(4) . . ? O24Y Cl21 O25Y 105.0(4) . . ? O22 Cl21 O25Y 107.9(3) . . ? O23X Cl21 O25Y 143.6(4) . . ? O24X Cl21 O25Y 86.7(4) . . ? O23Y Cl21 O25Y 98.3(4) . . ? O33 Cl31 O35 110.11(15) . . ? O33 Cl31 O34 109.95(13) . . ? O35 Cl31 O34 110.68(15) . . ? O33 Cl31 O32 107.76(15) . . ? O35 Cl31 O32 108.65(16) . . ? O34 Cl31 O32 109.63(14) . . ? C12S C11S H11A 109.5 . . ? C12S C11S H11B 109.5 . . ? H11A C11S H11B 109.5 . . ? C12S C11S H11C 109.5 . . ? H11A C11S H11C 109.5 . . ? H11B C11S H11C 109.5 . . ? N13S C12S C11S 178.9(5) . . ? C22S C21S H21A 109.5 . . ? C22S C21S H21B 109.5 . . ? H21A C21S H21B 109.5 . . ? C22S C21S H21C 109.5 . . ? H21A C21S H21C 109.5 . . ? H21B C21S H21C 109.5 . . ? N23S C22S C21S 178.7(5) . . ? _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N42A Ag1 Ag2 N22B -144.91(8) . . . . ? N11A Ag1 Ag2 N22B 52.19(8) . . . . ? N31A Ag1 Ag2 N22B 146.97(9) . . . . ? N22A Ag1 Ag2 N22B -11.46(8) . . . . ? N42A Ag1 Ag2 N31B 51.80(8) . . . . ? N11A Ag1 Ag2 N31B -111.11(8) . . . . ? N31A Ag1 Ag2 N31B -16.32(9) . . . . ? N22A Ag1 Ag2 N31B -174.76(8) . . . . ? N42A Ag1 Ag2 N11B 150.10(8) . . . . ? N11A Ag1 Ag2 N11B -12.80(8) . . . . ? N31A Ag1 Ag2 N11B 81.98(9) . . . . ? N22A Ag1 Ag2 N11B -76.45(8) . . . . ? N42A Ag1 Ag2 N42B -12.39(8) . . . . ? N11A Ag1 Ag2 N42B -175.29(8) . . . . ? N31A Ag1 Ag2 N42B -80.51(9) . . . . ? N22A Ag1 Ag2 N42B 121.06(8) . . . . ? N42A Ag1 N11A C12A 4.1(4) . . . . ? N31A Ag1 N11A C12A -46.3(2) . . . . ? N22A Ag1 N11A C12A -171.1(2) . . . . ? Ag2 Ag1 N11A C12A 67.9(2) . . . . ? N42A Ag1 N11A C16A -176.6(2) . . . . ? N31A Ag1 N11A C16A 133.1(2) . . . . ? N22A Ag1 N11A C16A 8.3(2) . . . . ? Ag2 Ag1 N11A C16A -112.7(2) . . . . ? C16A N11A C12A C13A 2.0(4) . . . . ? Ag1 N11A C12A C13A -178.6(2) . . . . ? N11A C12A C13A C14A -0.8(5) . . . . ? C12A C13A C14A C15A -0.7(4) . . . . ? C13A C14A C15A C16A 0.9(4) . . . . ? C12A N11A C16A C15A -1.7(4) . . . . ? Ag1 N11A C16A C15A 178.9(2) . . . . ? C12A N11A C16A C23A 178.3(2) . . . . ? Ag1 N11A C16A C23A -1.1(3) . . . . ? C14A C15A C16A N11A 0.3(4) . . . . ? C14A C15A C16A C23A -179.7(3) . . . . ? C25A N21A N22A C23A -0.1(3) . . . . ? C26A N21A N22A C23A -178.9(2) . . . . ? C25A N21A N22A Ag1 147.3(2) . . . . ? C26A N21A N22A Ag1 -31.5(4) . . . . ? N42A Ag1 N22A C23A 167.41(16) . . . . ? N11A Ag1 N22A C23A -14.63(17) . . . . ? N31A Ag1 N22A C23A -99.50(18) . . . . ? Ag2 Ag1 N22A C23A 56.42(18) . . . . ? N42A Ag1 N22A N21A 20.6(3) . . . . ? N11A Ag1 N22A N21A -161.4(3) . . . . ? N31A Ag1 N22A N21A 113.7(3) . . . . ? Ag2 Ag1 N22A N21A -90.4(3) . . . . ? N21A N22A C23A C24A -0.6(3) . . . . ? Ag1 N22A C23A C24A -160.1(2) . . . . ? N21A N22A C23A C16A 179.8(2) . . . . ? Ag1 N22A C23A C16A 20.3(3) . . . . ? N11A C16A C23A N22A -15.2(4) . . . . ? C15A C16A C23A N22A 164.8(3) . . . . ? N11A C16A C23A C24A 165.3(3) . . . . ? C15A C16A C23A C24A -14.7(5) . . . . ? N22A C23A C24A C25A 1.1(4) . . . . ? C16A C23A C24A C25A -179.4(3) . . . . ? N22A N21A C25A C24A 0.7(3) . . . . ? C26A N21A C25A C24A 179.4(3) . . . . ? C23A C24A C25A N21A -1.0(3) . . . . ? C25A N21A C26A C51A -110.5(3) . . . . ? N22A N21A C26A C51A 68.1(3) . . . . ? N42A Ag1 N31A C32A -179.5(3) . . . . ? N11A Ag1 N31A C32A -15.0(3) . . . . ? N22A Ag1 N31A C32A 55.8(3) . . . . ? Ag2 Ag1 N31A C32A -100.4(2) . . . . ? N42A Ag1 N31A C36A 8.80(19) . . . . ? N11A Ag1 N31A C36A 173.3(2) . . . . ? N22A Ag1 N31A C36A -115.95(19) . . . . ? Ag2 Ag1 N31A C36A 87.89(19) . . . . ? C36A N31A C32A C33A 1.0(4) . . . . ? Ag1 N31A C32A C33A -170.3(2) . . . . ? N31A C32A C33A C34A -0.4(5) . . . . ? C32A C33A C34A C35A -0.4(5) . . . . ? C33A C34A C35A C36A 0.5(5) . . . . ? C32A N31A C36A C35A -1.0(4) . . . . ? Ag1 N31A C36A C35A 171.7(2) . . . . ? C32A N31A C36A C43A -178.1(2) . . . . ? Ag1 N31A C36A C43A -5.4(3) . . . . ? C34A C35A C36A N31A 0.2(5) . . . . ? C34A C35A C36A C43A 177.2(3) . . . . ? C45A N41A N42A C43A 0.5(3) . . . . ? C46A N41A N42A C43A -179.1(2) . . . . ? C45A N41A N42A Ag1 161.6(2) . . . . ? C46A N41A N42A Ag1 -18.0(4) . . . . ? N11A Ag1 N42A C43A -65.5(4) . . . . ? N31A Ag1 N42A C43A -11.56(19) . . . . ? N22A Ag1 N42A C43A 108.6(2) . . . . ? Ag2 Ag1 N42A C43A -128.5(2) . . . . ? N11A Ag1 N42A N41A 135.4(3) . . . . ? N31A Ag1 N42A N41A -170.7(3) . . . . ? N22A Ag1 N42A N41A -50.5(3) . . . . ? Ag2 Ag1 N42A N41A 72.4(2) . . . . ? N41A N42A C43A C44A 0.0(3) . . . . ? Ag1 N42A C43A C44A -164.4(2) . . . . ? N41A N42A C43A C36A 178.0(2) . . . . ? Ag1 N42A C43A C36A 13.6(3) . . . . ? N31A C36A C43A N42A -4.6(4) . . . . ? C35A C36A C43A N42A 178.3(3) . . . . ? N31A C36A C43A C44A 173.0(3) . . . . ? C35A C36A C43A C44A -4.1(5) . . . . ? N42A C43A C44A C45A -0.5(3) . . . . ? C36A C43A C44A C45A -178.3(3) . . . . ? N42A N41A C45A C44A -0.8(3) . . . . ? C46A N41A C45A C44A 178.7(3) . . . . ? C43A C44A C45A N41A 0.8(3) . . . . ? C45A N41A C46A C54A -98.6(3) . . . . ? N42A N41A C46A C54A 80.9(3) . . . . ? N21A C26A C51A C52A 111.8(4) . . . . ? N21A C26A C51A O55A -68.2(3) . . . . ? O55A C51A C52A C53A 0.1(3) . . . . ? C26A C51A C52A C53A -179.9(3) . . . . ? C51A C52A C53A C54A 0.4(3) . . . . ? C52A C53A C54A O55A -0.9(3) . . . . ? C52A C53A C54A C46A 170.8(3) . . . . ? N41A C46A C54A C53A 145.2(3) . . . . ? N41A C46A C54A O55A -43.5(3) . . . . ? C53A C54A O55A C51A 0.9(3) . . . . ? C46A C54A O55A C51A -172.4(2) . . . . ? C52A C51A O55A C54A -0.6(3) . . . . ? C26A C51A O55A C54A 179.4(2) . . . . ? N22B Ag2 N11B C16B -1.10(19) . . . . ? N31B Ag2 N11B C16B 151.32(19) . . . . ? N42B Ag2 N11B C16B -134.91(19) . . . . ? Ag1 Ag2 N11B C16B 69.4(2) . . . . ? N22B Ag2 N11B C12B 178.9(2) . . . . ? N31B Ag2 N11B C12B -28.6(2) . . . . ? N42B Ag2 N11B C12B 45.1(3) . . . . ? Ag1 Ag2 N11B C12B -110.6(2) . . . . ? C16B N11B C12B C13B 0.7(4) . . . . ? Ag2 N11B C12B C13B -179.4(2) . . . . ? N11B C12B C13B C14B -2.5(5) . . . . ? C12B C13B C14B C15B 2.0(5) . . . . ? C13B C14B C15B C16B 0.1(5) . . . . ? C12B N11B C16B C15B 1.6(4) . . . . ? Ag2 N11B C16B C15B -178.4(2) . . . . ? C12B N11B C16B C23B -176.2(2) . . . . ? Ag2 N11B C16B C23B 3.8(3) . . . . ? C14B C15B C16B N11B -2.0(4) . . . . ? C14B C15B C16B C23B 175.8(3) . . . . ? C25B N21B N22B C23B 0.2(3) . . . . ? C26B N21B N22B C23B -179.2(2) . . . . ? C25B N21B N22B Ag2 168.6(2) . . . . ? C26B N21B N22B Ag2 -10.8(4) . . . . ? N31B Ag2 N22B C23B -80.7(3) . . . . ? N11B Ag2 N22B C23B -2.02(19) . . . . ? N42B Ag2 N22B C23B 134.82(18) . . . . ? Ag1 Ag2 N22B C23B -118.23(19) . . . . ? N31B Ag2 N22B N21B 111.8(3) . . . . ? N11B Ag2 N22B N21B -169.5(3) . . . . ? N42B Ag2 N22B N21B -32.6(3) . . . . ? Ag1 Ag2 N22B N21B 74.3(3) . . . . ? N21B N22B C23B C24B -0.6(3) . . . . ? Ag2 N22B C23B C24B -172.08(19) . . . . ? N21B N22B C23B C16B 176.3(2) . . . . ? Ag2 N22B C23B C16B 4.8(3) . . . . ? N11B C16B C23B N22B -5.9(4) . . . . ? C15B C16B C23B N22B 176.3(3) . . . . ? N11B C16B C23B C24B 170.4(3) . . . . ? C15B C16B C23B C24B -7.4(5) . . . . ? N22B C23B C24B C25B 0.7(3) . . . . ? C16B C23B C24B C25B -175.8(3) . . . . ? N22B N21B C25B C24B 0.2(3) . . . . ? C26B N21B C25B C24B 179.6(3) . . . . ? C23B C24B C25B N21B -0.6(3) . . . . ? C25B N21B C26B C51B -108.2(3) . . . . ? N22B N21B C26B C51B 71.1(3) . . . . ? N22B Ag2 N31B C36B -140.6(2) . . . . ? N11B Ag2 N31B C36B 148.2(2) . . . . ? N42B Ag2 N31B C36B 12.80(19) . . . . ? Ag1 Ag2 N31B C36B -102.9(2) . . . . ? N22B Ag2 N31B C32B 36.0(3) . . . . ? N11B Ag2 N31B C32B -35.2(2) . . . . ? N42B Ag2 N31B C32B -170.6(2) . . . . ? Ag1 Ag2 N31B C32B 73.7(2) . . . . ? C36B N31B C32B C33B 2.1(4) . . . . ? Ag2 N31B C32B C33B -174.5(2) . . . . ? N31B C32B C33B C34B 0.0(5) . . . . ? C32B C33B C34B C35B -1.6(5) . . . . ? C33B C34B C35B C36B 1.1(5) . . . . ? C32B N31B C36B C35B -2.6(4) . . . . ? Ag2 N31B C36B C35B 174.2(2) . . . . ? C32B N31B C36B C43B 177.0(2) . . . . ? Ag2 N31B C36B C43B -6.1(3) . . . . ? C34B C35B C36B N31B 1.1(5) . . . . ? C34B C35B C36B C43B -178.6(3) . . . . ? C45B N41B N42B C43B 1.1(3) . . . . ? C46B N41B N42B C43B 178.1(2) . . . . ? C45B N41B N42B Ag2 148.8(2) . . . . ? C46B N41B N42B Ag2 -34.1(4) . . . . ? N22B Ag2 N42B C43B 145.21(17) . . . . ? N31B Ag2 N42B C43B -18.22(18) . . . . ? N11B Ag2 N42B C43B -104.7(2) . . . . ? Ag1 Ag2 N42B C43B 51.22(19) . . . . ? N22B Ag2 N42B N41B -1.3(3) . . . . ? N31B Ag2 N42B N41B -164.7(3) . . . . ? N11B Ag2 N42B N41B 108.9(3) . . . . ? Ag1 Ag2 N42B N41B -95.2(3) . . . . ? N41B N42B C43B C44B -1.1(3) . . . . ? Ag2 N42B C43B C44B -158.38(19) . . . . ? N41B N42B C43B C36B -179.7(2) . . . . ? Ag2 N42B C43B C36B 23.0(3) . . . . ? N31B C36B C43B N42B -12.6(4) . . . . ? C35B C36B C43B N42B 167.1(3) . . . . ? N31B C36B C43B C44B 169.1(3) . . . . ? C35B C36B C43B C44B -11.3(5) . . . . ? N42B C43B C44B C45B 0.6(3) . . . . ? C36B C43B C44B C45B 179.1(3) . . . . ? N42B N41B C45B C44B -0.7(3) . . . . ? C46B N41B C45B C44B -177.5(3) . . . . ? C43B C44B C45B N41B 0.0(3) . . . . ? C45B N41B C46B C54B -107.4(3) . . . . ? N42B N41B C46B C54B 76.1(3) . . . . ? N21B C26B C51B C52B 122.3(4) . . . . ? N21B C26B C51B O55B -61.9(3) . . . . ? O55B C51B C52B C53B -1.1(4) . . . . ? C26B C51B C52B C53B 174.8(3) . . . . ? C51B C52B C53B C54B 0.8(4) . . . . ? C52B C53B C54B O55B -0.2(4) . . . . ? C52B C53B C54B C46B 174.5(3) . . . . ? N41B C46B C54B C53B 134.4(4) . . . . ? N41B C46B C54B O55B -51.1(4) . . . . ? C53B C54B O55B C51B -0.5(3) . . . . ? C46B C54B O55B C51B -176.3(2) . . . . ? C52B C51B O55B C54B 1.0(3) . . . . ? C26B C51B O55B C54B -175.8(2) . . . . ? N42C Ag3 N11C C12C -15.3(3) . . . . ? N22C Ag3 N11C C12C 174.1(2) . . . . ? N31C Ag3 N11C C12C 41.7(2) . . . . ? N42C Ag3 N11C C16C 176.57(18) . . . . ? N22C Ag3 N11C C16C 6.00(19) . . . . ? N31C Ag3 N11C C16C -126.3(2) . . . . ? C16C N11C C12C C13C 0.6(4) . . . . ? Ag3 N11C C12C C13C -167.4(2) . . . . ? N11C C12C C13C C14C 0.4(5) . . . . ? C12C C13C C14C C15C -1.3(5) . . . . ? C13C C14C C15C C16C 1.3(5) . . . . ? C12C N11C C16C C15C -0.6(4) . . . . ? Ag3 N11C C16C C15C 168.2(2) . . . . ? C12C N11C C16C C23C 179.5(2) . . . . ? Ag3 N11C C16C C23C -11.6(3) . . . . ? C14C C15C C16C N11C -0.3(4) . . . . ? C14C C15C C16C C23C 179.5(3) . . . . ? C25C N21C N22C C23C -1.6(3) . . . . ? C26C N21C N22C C23C -173.9(2) . . . . ? C25C N21C N22C Ag3 -169.4(2) . . . . ? C26C N21C N22C Ag3 18.3(4) . . . . ? N42C Ag3 N22C C23C -172.72(17) . . . . ? N11C Ag3 N22C C23C 0.59(18) . . . . ? N31C Ag3 N22C C23C 80.0(2) . . . . ? N42C Ag3 N22C N21C -5.6(3) . . . . ? N11C Ag3 N22C N21C 167.7(3) . . . . ? N31C Ag3 N22C N21C -112.9(3) . . . . ? N21C N22C C23C C24C 1.3(3) . . . . ? Ag3 N22C C23C C24C 173.08(18) . . . . ? N21C N22C C23C C16C -178.6(2) . . . . ? Ag3 N22C C23C C16C -6.8(3) . . . . ? N11C C16C C23C N22C 12.6(4) . . . . ? C15C C16C C23C N22C -167.3(3) . . . . ? N11C C16C C23C C24C -167.3(3) . . . . ? C15C C16C C23C C24C 12.8(5) . . . . ? N22C C23C C24C C25C -0.6(3) . . . . ? C16C C23C C24C C25C 179.2(3) . . . . ? N22C N21C C25C C24C 1.2(3) . . . . ? C26C N21C C25C C24C 173.0(3) . . . . ? C23C C24C C25C N21C -0.3(3) . . . . ? C25C N21C C26C C51C 128.4(3) . . . . ? N22C N21C C26C C51C -60.4(4) . . . . ? N42C Ag3 N31C C36C -2.9(2) . . . . ? N11C Ag3 N31C C36C -157.3(2) . . . . ? N22C Ag3 N31C C36C 133.50(19) . . . . ? N42C Ag3 N31C C32C 171.9(3) . . . . ? N11C Ag3 N31C C32C 17.5(3) . . . . ? N22C Ag3 N31C C32C -51.8(3) . . . . ? C36C N31C C32C C33C -1.2(5) . . . . ? Ag3 N31C C32C C33C -175.7(2) . . . . ? N31C C32C C33C C34C 0.7(5) . . . . ? C32C C33C C34C C35C 0.4(5) . . . . ? C33C C34C C35C C36C -0.9(5) . . . . ? C32C N31C C36C C35C 0.6(4) . . . . ? Ag3 N31C C36C C35C 176.0(2) . . . . ? C32C N31C C36C C43C -178.1(3) . . . . ? Ag3 N31C C36C C43C -2.7(3) . . . . ? C34C C35C C36C N31C 0.4(5) . . . . ? C34C C35C C36C C43C 179.1(3) . . . . ? C45C N41C N42C C43C -0.3(3) . . . . ? C46C N41C N42C C43C -176.0(3) . . . . ? C45C N41C N42C Ag3 -161.4(2) . . . . ? C46C N41C N42C Ag3 22.9(4) . . . . ? N11C Ag3 N42C N41C -129.6(3) . . . . ? N22C Ag3 N42C N41C 37.3(3) . . . . ? N31C Ag3 N42C N41C 167.9(3) . . . . ? N11C Ag3 N42C C43C 71.2(3) . . . . ? N22C Ag3 N42C C43C -122.0(2) . . . . ? N31C Ag3 N42C C43C 8.6(2) . . . . ? N41C N42C C43C C44C 0.4(3) . . . . ? Ag3 N42C C43C C44C 165.2(2) . . . . ? N41C N42C C43C C36C -178.8(3) . . . . ? Ag3 N42C C43C C36C -14.0(4) . . . . ? N31C C36C C43C N42C 11.0(4) . . . . ? C35C C36C C43C N42C -167.8(3) . . . . ? N31C C36C C43C C44C -168.0(3) . . . . ? C35C C36C C43C C44C 13.3(5) . . . . ? N42C C43C C44C C45C -0.4(4) . . . . ? C36C C43C C44C C45C 178.7(3) . . . . ? N42C N41C C45C C44C 0.0(4) . . . . ? C46C N41C C45C C44C 175.3(3) . . . . ? C43C C44C C45C N41C 0.2(4) . . . . ? N42C N41C C46C C54C -75.9(4) . . . . ? C45C N41C C46C C54C 109.2(4) . . . . ? N21C C26C C51C C52C -132.5(3) . . . . ? N21C C26C C51C O55C 57.6(4) . . . . ? O55C C51C C52C C53C 0.6(3) . . . . ? C26C C51C C52C C53C -170.0(3) . . . . ? C51C C52C C53C C54C -0.7(4) . . . . ? C52C C53C C54C O55C 0.6(4) . . . . ? C52C C53C C54C C46C -174.3(3) . . . . ? N41C C46C C54C C53C -133.5(4) . . . . ? N41C C46C C54C O55C 51.8(4) . . . . ? C52C C51C O55C C54C -0.2(3) . . . . ? C26C C51C O55C C54C 171.9(2) . . . . ? C53C C54C O55C C51C -0.3(3) . . . . ? C46C C54C O55C C51C 175.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.803 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.206 data_imw1463 _database_code_depnum_ccdc_archive 'CCDC 895599' #TrackingRef 'Ag_Ward_Stephenson_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H36 Ag2 Cl2 N12 O8 S2' _chemical_formula_weight 1211.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pca2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 18.5223(9) _cell_length_b 11.5704(6) _cell_length_c 21.6258(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4634.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9614 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.30 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 1.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8963 _exptl_absorpt_correction_T_max 0.9462 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 86041 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.72 _reflns_number_total 10768 _reflns_number_gt 8691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. The hydrogens were all added in calculated positions. The two perchlorate counter ions both have complete disorder around the respective chlorine atoms (both 50:50). The perchlorates have been left isotropic due to their disorder and fluxional nature The possibilty of local inversion symmetry was detected and dealt with using the 'TWIN BASF 0.5' command which solved the problem 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^)+(0.0504P)^2^+5.4150P] 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 0.40(2) _refine_ls_number_reflns 10768 _refine_ls_number_parameters 616 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.638711(17) 0.26527(3) 0.808481(19) 0.03146(9) Uani 1 1 d . . . Ag2 Ag 0.173356(18) 0.26322(3) 0.80928(2) 0.03464(9) Uani 1 1 d . . . N11A N 0.64646(19) 0.1319(3) 0.73477(17) 0.0242(8) Uani 1 1 d . . . C12A C 0.6835(2) 0.1481(4) 0.6821(2) 0.0289(10) Uani 1 1 d . . . H12A H 0.7178 0.2091 0.6806 0.035 Uiso 1 1 calc R . . C13A C 0.6743(3) 0.0809(5) 0.6302(2) 0.0361(11) Uani 1 1 d . . . H13A H 0.7014 0.0957 0.5938 0.043 Uiso 1 1 calc R . . C14A C 0.6247(3) -0.0089(4) 0.6321(2) 0.0347(11) Uani 1 1 d . . . H14A H 0.6173 -0.0570 0.5971 0.042 Uiso 1 1 calc R . . C15A C 0.5862(2) -0.0269(4) 0.6861(2) 0.0289(10) Uani 1 1 d . . . H15A H 0.5518 -0.0877 0.6885 0.035 Uiso 1 1 calc R . . C16A C 0.5980(2) 0.0443(4) 0.73709(19) 0.0213(8) Uani 1 1 d . . . N21A N 0.51480(19) 0.0639(3) 0.88406(16) 0.0253(8) Uani 1 1 d . . . N22A N 0.55898(19) 0.1055(3) 0.84016(16) 0.0237(7) Uani 1 1 d . . . C23A C 0.5560(2) 0.0274(4) 0.79428(18) 0.0244(9) Uani 1 1 d . . . C24A C 0.5102(2) -0.0643(3) 0.8092(3) 0.0304(9) Uani 1 1 d . . . H24A H 0.4995 -0.1304 0.7849 0.037 Uiso 1 1 calc R . . C25A C 0.4841(3) -0.0380(4) 0.8669(2) 0.0326(10) Uani 1 1 d . . . H25A H 0.4508 -0.0824 0.8904 0.039 Uiso 1 1 calc R . . C26A C 0.5022(2) 0.1283(4) 0.9417(2) 0.0289(10) Uani 1 1 d . . . H26A H 0.5427 0.1826 0.9484 0.035 Uiso 1 1 calc R . . H26B H 0.5015 0.0733 0.9768 0.035 Uiso 1 1 calc R . . N31A N 0.1603(2) 0.3651(3) 0.71662(18) 0.0272(8) Uani 1 1 d . . . C32A C 0.1209(3) 0.3319(4) 0.6679(2) 0.0319(10) Uani 1 1 d . . . H32A H 0.0877 0.2702 0.6733 0.038 Uiso 1 1 calc R . . C33A C 0.1262(3) 0.3831(5) 0.6095(2) 0.0381(12) Uani 1 1 d . . . H33A H 0.0978 0.3564 0.5758 0.046 Uiso 1 1 calc R . . C34A C 0.1743(3) 0.4745(5) 0.6023(2) 0.0392(12) Uani 1 1 d . . . H34A H 0.1799 0.5109 0.5632 0.047 Uiso 1 1 calc R . . C35A C 0.2136(3) 0.5111(4) 0.6522(2) 0.0346(11) Uani 1 1 d . . . H35A H 0.2461 0.5742 0.6480 0.042 Uiso 1 1 calc R . . C36A C 0.2060(2) 0.4561(4) 0.7093(2) 0.0262(9) Uani 1 1 d . . . N41A N 0.2867(2) 0.4898(3) 0.85641(17) 0.0256(8) Uani 1 1 d . . . N42A N 0.24346(19) 0.4326(3) 0.8158(2) 0.0268(8) Uani 1 1 d . . . C43A C 0.2468(2) 0.4947(4) 0.7635(2) 0.0249(9) Uani 1 1 d . . . C44A C 0.2918(3) 0.5910(4) 0.7707(2) 0.0303(11) Uani 1 1 d . . . H44A H 0.3033 0.6477 0.7405 0.036 Uiso 1 1 calc R . . C45A C 0.3158(3) 0.5860(4) 0.8311(2) 0.0310(11) Uani 1 1 d . . . H45A H 0.3468 0.6397 0.8510 0.037 Uiso 1 1 calc R . . C46A C 0.2932(3) 0.4498(4) 0.9202(2) 0.0295(10) Uani 1 1 d . . . H46A H 0.2440 0.4369 0.9368 0.035 Uiso 1 1 calc R . . H46B H 0.3156 0.5122 0.9450 0.035 Uiso 1 1 calc R . . C51A C 0.4331(2) 0.1947(4) 0.9413(2) 0.0257(9) Uani 1 1 d . . . C52A C 0.3687(2) 0.1610(4) 0.96694(19) 0.0270(9) Uani 1 1 d . . . H52A H 0.3617 0.0886 0.9867 0.032 Uiso 1 1 calc R . . C53A C 0.3138(2) 0.2456(4) 0.9608(2) 0.0253(9) Uani 1 1 d . . . H53A H 0.2664 0.2364 0.9768 0.030 Uiso 1 1 calc R . . C54A C 0.3362(2) 0.3417(4) 0.92956(19) 0.0247(9) Uani 1 1 d . . . S55A S 0.42497(6) 0.32945(10) 0.90810(6) 0.0323(3) Uani 1 1 d . . . N11B N 0.64362(19) 0.3757(3) 0.89488(17) 0.0239(8) Uani 1 1 d . . . C12B C 0.6764(2) 0.3421(4) 0.9470(2) 0.0288(10) Uani 1 1 d . . . H12B H 0.7112 0.2820 0.9444 0.035 Uiso 1 1 calc R . . C13B C 0.6628(3) 0.3892(4) 1.0037(2) 0.0336(11) Uani 1 1 d . . . H13B H 0.6885 0.3638 1.0392 0.040 Uiso 1 1 calc R . . C14B C 0.6112(3) 0.4742(5) 1.0083(2) 0.0391(12) Uani 1 1 d . . . H14B H 0.5999 0.5069 1.0474 0.047 Uiso 1 1 calc R . . C15B C 0.5762(3) 0.5117(4) 0.9558(2) 0.0332(11) Uani 1 1 d . . . H15B H 0.5406 0.5707 0.9581 0.040 Uiso 1 1 calc R . . C16B C 0.5939(2) 0.4610(4) 0.8989(2) 0.0231(9) Uani 1 1 d . . . N21B N 0.51839(19) 0.4769(3) 0.74917(17) 0.0269(8) Uani 1 1 d . . . N22B N 0.55990(19) 0.4259(3) 0.79248(16) 0.0250(8) Uani 1 1 d . . . C23B C 0.5563(2) 0.4951(4) 0.8418(2) 0.0231(9) Uani 1 1 d . . . C24B C 0.5123(3) 0.5909(4) 0.8295(2) 0.0308(11) Uani 1 1 d . . . H24B H 0.5009 0.6528 0.8566 0.037 Uiso 1 1 calc R . . C25B C 0.4892(2) 0.5760(4) 0.7701(2) 0.0286(10) Uani 1 1 d . . . H25B H 0.4583 0.6263 0.7476 0.034 Uiso 1 1 calc R . . C26B C 0.5084(3) 0.4230(4) 0.6884(2) 0.0308(10) Uani 1 1 d . . . H26C H 0.5566 0.4064 0.6708 0.037 Uiso 1 1 calc R . . H26D H 0.4845 0.4796 0.6609 0.037 Uiso 1 1 calc R . . N31B N 0.1537(2) 0.1506(3) 0.89564(17) 0.0267(8) Uani 1 1 d . . . C32B C 0.1102(3) 0.1790(4) 0.9427(2) 0.0329(10) Uani 1 1 d . . . H32B H 0.0780 0.2421 0.9369 0.039 Uiso 1 1 calc R . . C33B C 0.1089(3) 0.1224(5) 0.9992(2) 0.0386(12) Uani 1 1 d . . . H33B H 0.0780 0.1472 1.0317 0.046 Uiso 1 1 calc R . . C34B C 0.1544(3) 0.0283(5) 1.0064(2) 0.0386(12) Uani 1 1 d . . . H34B H 0.1548 -0.0133 1.0443 0.046 Uiso 1 1 calc R . . C35B C 0.1990(3) -0.0048(4) 0.9588(2) 0.0347(11) Uani 1 1 d . . . H35B H 0.2301 -0.0694 0.9633 0.042 Uiso 1 1 calc R . . C36B C 0.1979(2) 0.0580(4) 0.9034(2) 0.0277(9) Uani 1 1 d . . . N41B N 0.2920(2) 0.0417(4) 0.76162(19) 0.0324(9) Uani 1 1 d . . . N42B N 0.24451(19) 0.0928(3) 0.80000(19) 0.0290(8) Uani 1 1 d . . . C43B C 0.2443(3) 0.0270(4) 0.8508(2) 0.0278(10) Uani 1 1 d . . . C44B C 0.2913(3) -0.0670(5) 0.8452(3) 0.0379(12) Uani 1 1 d . . . H44B H 0.3010 -0.1257 0.8748 0.046 Uiso 1 1 calc R . . C45B C 0.3206(3) -0.0547(5) 0.7863(3) 0.0413(13) Uani 1 1 d . . . H45B H 0.3545 -0.1049 0.7671 0.050 Uiso 1 1 calc R . . C46B C 0.3043(3) 0.0913(5) 0.6998(2) 0.0387(12) Uani 1 1 d . . . H46C H 0.2622 0.1401 0.6890 0.046 Uiso 1 1 calc R . . H46D H 0.3062 0.0272 0.6695 0.046 Uiso 1 1 calc R . . C51B C 0.4657(3) 0.3147(4) 0.6877(2) 0.0314(10) Uani 1 1 d . . . C52B C 0.4864(3) 0.2154(4) 0.6605(2) 0.0328(10) Uani 1 1 d . . . H52B H 0.5321 0.2053 0.6412 0.039 Uiso 1 1 calc R . . C53B C 0.4332(3) 0.1275(4) 0.6634(2) 0.0328(10) Uani 1 1 d . . . H53B H 0.4398 0.0523 0.6467 0.039 Uiso 1 1 calc R . . C54B C 0.3710(3) 0.1622(4) 0.6928(2) 0.0358(11) Uani 1 1 d . . . S55B S 0.38070(7) 0.30375(13) 0.71865(7) 0.0415(3) Uani 1 1 d . . . Cl11 Cl 0.40980(5) 0.76846(9) 0.63390(5) 0.0230(2) Uiso 1 1 d . . . O12X O 0.4412(8) 0.8152(11) 0.6896(6) 0.042(4) Uiso 0.50(4) 1 d P A 1 O13X O 0.3458(7) 0.8302(12) 0.6166(6) 0.039(3) Uiso 0.50(4) 1 d P A 1 O14X O 0.3910(8) 0.6455(5) 0.6416(4) 0.020(3) Uiso 0.50(4) 1 d P A 1 O15X O 0.4621(5) 0.7785(16) 0.5859(5) 0.043(3) Uiso 0.50(4) 1 d P A 1 O12Y O 0.4289(6) 0.8076(8) 0.6958(4) 0.018(3) Uiso 0.50(4) 1 d P A 2 O13Y O 0.3370(6) 0.8099(11) 0.6229(5) 0.031(3) Uiso 0.50(4) 1 d P A 2 O14Y O 0.4141(10) 0.6461(7) 0.6335(5) 0.038(3) Uiso 0.50(4) 1 d P A 2 O15Y O 0.4598(5) 0.8153(15) 0.5902(4) 0.038(3) Uiso 0.50(4) 1 d P A 2 Cl21 Cl 0.39800(6) 0.75371(9) 0.99440(5) 0.0258(2) Uiso 1 1 d . . . O22X O 0.4242(12) 0.6779(16) 1.0396(9) 0.110(6) Uiso 0.50(2) 1 d P B 1 O23X O 0.3274(4) 0.7190(9) 1.0110(4) 0.034(2) Uiso 0.50(2) 1 d P B 1 O24X O 0.4294(7) 0.8640(7) 1.0126(4) 0.034(2) Uiso 0.50(2) 1 d P B 1 O25X O 0.4251(6) 0.7091(9) 0.9371(5) 0.041(3) Uiso 0.50(2) 1 d P B 1 O22Y O 0.4471(6) 0.6833(8) 1.0302(4) 0.042(3) Uiso 0.50(2) 1 d P B 2 O23Y O 0.3195(8) 0.7519(15) 0.9990(8) 0.077(4) Uiso 0.50(2) 1 d P B 2 O24Y O 0.4060(6) 0.8779(7) 0.9999(4) 0.029(2) Uiso 0.50(2) 1 d P B 2 O25Y O 0.4069(6) 0.7328(9) 0.9278(4) 0.037(2) Uiso 0.50(2) 1 d P 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 0.03368(17) 0.02537(15) 0.03533(17) -0.0074(2) -0.0003(2) -0.00099(12) Ag2 0.04036(19) 0.02930(16) 0.03427(17) 0.0070(2) 0.0037(2) -0.00301(13) N11A 0.0199(18) 0.0238(19) 0.0288(19) 0.0018(15) -0.0011(15) 0.0039(15) C12A 0.025(2) 0.031(2) 0.030(2) 0.0060(19) 0.0026(19) 0.0047(18) C13A 0.033(3) 0.045(3) 0.030(3) 0.010(2) 0.006(2) 0.009(2) C14A 0.041(3) 0.040(3) 0.023(2) -0.006(2) -0.002(2) 0.008(2) C15A 0.032(2) 0.028(2) 0.027(2) -0.0048(18) -0.0013(19) 0.0041(19) C16A 0.020(2) 0.021(2) 0.023(2) 0.0021(16) -0.0066(16) 0.0041(16) N21A 0.0231(19) 0.030(2) 0.0232(18) -0.0010(15) 0.0004(15) 0.0000(15) N22A 0.0238(18) 0.0263(19) 0.0210(17) 0.0006(15) 0.0010(15) 0.0028(15) C23A 0.023(2) 0.028(2) 0.022(2) 0.0003(16) -0.0045(16) 0.0048(17) C24A 0.031(2) 0.030(2) 0.030(2) -0.002(3) -0.011(2) -0.0026(16) C25A 0.031(2) 0.034(2) 0.033(2) 0.003(2) 0.001(2) -0.008(2) C26A 0.023(2) 0.041(3) 0.023(2) 0.0025(19) -0.0006(18) 0.004(2) N31A 0.0254(19) 0.0271(19) 0.029(2) -0.0012(16) 0.0023(16) 0.0031(15) C32A 0.031(3) 0.030(2) 0.034(3) 0.000(2) -0.001(2) 0.003(2) C33A 0.046(3) 0.038(3) 0.031(3) -0.008(2) -0.004(2) 0.006(2) C34A 0.052(3) 0.045(3) 0.020(2) 0.003(2) 0.002(2) 0.005(2) C35A 0.042(3) 0.031(2) 0.030(2) 0.0021(19) 0.003(2) -0.001(2) C36A 0.024(2) 0.026(2) 0.028(2) -0.0007(18) 0.0076(18) 0.0048(17) N41A 0.0263(19) 0.0243(19) 0.026(2) 0.0024(15) 0.0002(16) 0.0040(16) N42A 0.0261(18) 0.0248(16) 0.029(2) -0.0044(18) 0.0016(17) 0.0025(13) C43A 0.022(2) 0.023(2) 0.029(2) 0.0005(17) 0.0081(19) 0.0023(18) C44A 0.029(3) 0.032(3) 0.030(2) 0.0045(19) 0.006(2) 0.000(2) C45A 0.028(2) 0.029(2) 0.035(3) 0.0027(19) 0.000(2) 0.000(2) C46A 0.037(3) 0.025(2) 0.026(2) -0.0046(18) -0.001(2) 0.0029(19) C51A 0.021(2) 0.028(2) 0.028(2) 0.0023(18) -0.0030(18) 0.0016(18) C52A 0.026(2) 0.034(2) 0.021(2) 0.0009(18) 0.0006(18) -0.0034(18) C53A 0.023(2) 0.031(2) 0.022(2) 0.0007(17) 0.0047(17) -0.0019(17) C54A 0.022(2) 0.030(2) 0.023(2) -0.0039(17) -0.0023(17) 0.0027(17) S55A 0.0266(6) 0.0326(6) 0.0376(6) 0.0080(5) 0.0065(5) -0.0015(5) N11B 0.0220(18) 0.0227(18) 0.027(2) 0.0017(15) -0.0009(15) -0.0058(14) C12B 0.027(2) 0.027(2) 0.033(3) 0.0056(19) -0.0030(19) -0.0047(18) C13B 0.039(3) 0.036(3) 0.026(2) 0.009(2) -0.004(2) -0.006(2) C14B 0.054(3) 0.040(3) 0.023(2) 0.001(2) 0.007(2) -0.008(2) C15B 0.035(3) 0.034(3) 0.030(3) 0.006(2) 0.003(2) -0.002(2) C16B 0.024(2) 0.0193(19) 0.027(2) 0.0035(16) -0.0001(18) -0.0040(16) N21B 0.0265(19) 0.0270(19) 0.027(2) 0.0041(15) 0.0013(16) -0.0002(15) N22B 0.0221(18) 0.0266(18) 0.026(2) 0.0042(14) -0.0012(14) 0.0001(14) C23B 0.019(2) 0.023(2) 0.027(2) 0.0006(17) 0.0046(17) -0.0032(17) C24B 0.032(3) 0.025(2) 0.035(3) 0.0007(18) 0.006(2) 0.0053(19) C25B 0.024(2) 0.029(2) 0.033(2) 0.0066(19) -0.0006(19) 0.0007(19) C26B 0.030(2) 0.039(3) 0.023(2) 0.0010(19) -0.0019(19) 0.002(2) N31B 0.0218(18) 0.0291(19) 0.029(2) 0.0015(16) -0.0017(16) -0.0048(15) C32B 0.029(2) 0.035(3) 0.035(3) 0.002(2) 0.002(2) 0.001(2) C33B 0.034(3) 0.051(3) 0.031(3) 0.002(2) 0.004(2) -0.010(2) C34B 0.041(3) 0.043(3) 0.032(3) 0.007(2) -0.002(2) -0.014(2) C35B 0.044(3) 0.025(2) 0.035(3) 0.007(2) -0.008(2) -0.008(2) C36B 0.025(2) 0.028(2) 0.030(2) -0.0002(18) -0.0051(19) -0.0043(17) N41B 0.022(2) 0.040(2) 0.035(2) -0.0149(18) 0.0010(17) -0.0045(17) N42B 0.0243(18) 0.0335(19) 0.029(2) -0.0090(18) 0.0009(17) -0.0048(14) C43B 0.028(2) 0.024(2) 0.031(3) -0.0073(18) -0.0056(19) -0.0036(19) C44B 0.036(3) 0.039(3) 0.039(3) -0.003(2) -0.007(2) 0.004(2) C45B 0.033(3) 0.041(3) 0.050(3) -0.014(2) -0.004(2) 0.007(2) C46B 0.035(3) 0.054(3) 0.027(2) -0.011(2) 0.004(2) -0.006(2) C51B 0.032(3) 0.039(3) 0.023(2) 0.001(2) 0.0041(19) 0.006(2) C52B 0.035(3) 0.039(3) 0.024(2) 0.000(2) 0.0006(19) 0.005(2) C53B 0.033(2) 0.036(3) 0.030(2) -0.005(2) -0.003(2) 0.002(2) C54B 0.047(3) 0.031(3) 0.029(2) -0.010(2) -0.002(2) -0.003(2) S55B 0.0290(6) 0.0450(7) 0.0504(8) -0.0167(6) 0.0058(6) 0.0009(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 N11A 2.223(4) . ? Ag1 N11B 2.265(4) . ? Ag1 N22B 2.389(4) . ? Ag1 N22A 2.463(4) . ? Ag2 N31B 2.306(4) . ? Ag2 N31A 2.338(4) . ? Ag2 N42A 2.355(4) . ? Ag2 N42B 2.380(4) . ? N11A C12A 1.342(6) . ? N11A C16A 1.355(5) . ? C12A C13A 1.376(7) . ? C12A H12A 0.9500 . ? C13A C14A 1.387(7) . ? C13A H13A 0.9500 . ? C14A C15A 1.384(7) . ? C14A H14A 0.9500 . ? C15A C16A 1.394(6) . ? C15A H15A 0.9500 . ? C16A C23A 1.474(6) . ? N21A N22A 1.343(5) . ? N21A C25A 1.360(6) . ? N21A C26A 1.471(6) . ? N22A C23A 1.343(5) . ? C23A C24A 1.396(6) . ? C24A C25A 1.372(7) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C26A C51A 1.492(6) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? N31A C32A 1.337(6) . ? N31A C36A 1.360(6) . ? C32A C33A 1.399(7) . ? C32A H32A 0.9500 . ? C33A C34A 1.392(8) . ? C33A H33A 0.9500 . ? C34A C35A 1.370(7) . ? C34A H34A 0.9500 . ? C35A C36A 1.397(7) . ? C35A H35A 0.9500 . ? C36A C43A 1.463(7) . ? N41A C45A 1.352(6) . ? N41A N42A 1.361(5) . ? N41A C46A 1.460(6) . ? N42A C43A 1.341(6) . ? C43A C44A 1.401(6) . ? C44A C45A 1.381(7) . ? C44A H44A 0.9500 . ? C45A H45A 0.9500 . ? C46A C54A 1.496(6) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C51A C52A 1.371(6) . ? C51A S55A 1.724(5) . ? C52A C53A 1.418(6) . ? C52A H52A 0.9500 . ? C53A C54A 1.366(6) . ? C53A H53A 0.9500 . ? C54A S55A 1.715(4) . ? N11B C12B 1.338(6) . ? N11B C16B 1.353(6) . ? C12B C13B 1.366(7) . ? C12B H12B 0.9500 . ? C13B C14B 1.375(7) . ? C13B H13B 0.9500 . ? C14B C15B 1.379(7) . ? C14B H14B 0.9500 . ? C15B C16B 1.401(6) . ? C15B H15B 0.9500 . ? C16B C23B 1.471(6) . ? N21B C25B 1.346(6) . ? N21B N22B 1.348(5) . ? N21B C26B 1.466(6) . ? N22B C23B 1.336(6) . ? C23B C24B 1.402(6) . ? C24B C25B 1.365(7) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B C51B 1.481(7) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? N31B C32B 1.339(6) . ? N31B C36B 1.359(6) . ? C32B C33B 1.387(7) . ? C32B H32B 0.9500 . ? C33B C34B 1.386(8) . ? C33B H33B 0.9500 . ? C34B C35B 1.375(7) . ? C34B H34B 0.9500 . ? C35B C36B 1.402(6) . ? C35B H35B 0.9500 . ? C36B C43B 1.468(7) . ? N41B C45B 1.345(7) . ? N41B N42B 1.347(5) . ? N41B C46B 1.472(6) . ? N42B C43B 1.337(6) . ? C43B C44B 1.399(7) . ? C44B C45B 1.392(7) . ? C44B H44B 0.9500 . ? C45B H45B 0.9500 . ? C46B C54B 1.492(7) . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C51B C52B 1.347(7) . ? C51B S55B 1.716(5) . ? C52B C53B 1.417(7) . ? C52B H52B 0.9500 . ? C53B C54B 1.376(7) . ? C53B H53B 0.9500 . ? C54B S55B 1.740(5) . ? Cl11 O14Y 1.418(8) . ? Cl11 O15X 1.424(10) . ? Cl11 O15Y 1.430(9) . ? Cl11 O13X 1.434(11) . ? Cl11 O12X 1.443(12) . ? Cl11 O13Y 1.451(10) . ? Cl11 O12Y 1.456(9) . ? Cl11 O14X 1.475(7) . ? Cl21 O22X 1.401(18) . ? Cl21 O23X 1.414(8) . ? Cl21 O25X 1.434(9) . ? Cl21 O22Y 1.446(9) . ? Cl21 O24Y 1.449(7) . ? Cl21 O24X 1.457(8) . ? Cl21 O23Y 1.458(14) . ? Cl21 O25Y 1.470(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 N11A Ag1 N11B 168.60(13) . . ? N11A Ag1 N22B 118.40(12) . . ? N11B Ag1 N22B 72.85(12) . . ? N11A Ag1 N22A 73.58(13) . . ? N11B Ag1 N22A 102.59(12) . . ? N22B Ag1 N22A 104.94(11) . . ? N31B Ag2 N31A 164.32(12) . . ? N31B Ag2 N42A 120.61(14) . . ? N31A Ag2 N42A 71.84(14) . . ? N31B Ag2 N42B 71.80(14) . . ? N31A Ag2 N42B 113.76(14) . . ? N42A Ag2 N42B 112.89(11) . . ? C12A N11A C16A 118.3(4) . . ? C12A N11A Ag1 123.0(3) . . ? C16A N11A Ag1 116.7(3) . . ? N11A C12A C13A 123.4(4) . . ? N11A C12A H12A 118.3 . . ? C13A C12A H12A 118.3 . . ? C12A C13A C14A 118.8(4) . . ? C12A C13A H13A 120.6 . . ? C14A C13A H13A 120.6 . . ? C15A C14A C13A 118.6(4) . . ? C15A C14A H14A 120.7 . . ? C13A C14A H14A 120.7 . . ? C14A C15A C16A 119.8(4) . . ? C14A C15A H15A 120.1 . . ? C16A C15A H15A 120.1 . . ? N11A C16A C15A 121.2(4) . . ? N11A C16A C23A 118.7(4) . . ? C15A C16A C23A 120.1(4) . . ? N22A N21A C25A 111.9(4) . . ? N22A N21A C26A 120.9(4) . . ? C25A N21A C26A 127.1(4) . . ? N21A N22A C23A 104.8(3) . . ? N21A N22A Ag1 146.2(3) . . ? C23A N22A Ag1 108.9(3) . . ? N22A C23A C24A 111.4(4) . . ? N22A C23A C16A 120.6(4) . . ? C24A C23A C16A 128.0(4) . . ? C25A C24A C23A 104.9(4) . . ? C25A C24A H24A 127.6 . . ? C23A C24A H24A 127.6 . . ? N21A C25A C24A 107.0(4) . . ? N21A C25A H25A 126.5 . . ? C24A C25A H25A 126.5 . . ? N21A C26A C51A 113.1(4) . . ? N21A C26A H26A 109.0 . . ? C51A C26A H26A 109.0 . . ? N21A C26A H26B 109.0 . . ? C51A C26A H26B 109.0 . . ? H26A C26A H26B 107.8 . . ? C32A N31A C36A 118.1(4) . . ? C32A N31A Ag2 125.9(3) . . ? C36A N31A Ag2 115.2(3) . . ? N31A C32A C33A 123.5(5) . . ? N31A C32A H32A 118.3 . . ? C33A C32A H32A 118.3 . . ? C34A C33A C32A 117.9(5) . . ? C34A C33A H33A 121.0 . . ? C32A C33A H33A 121.0 . . ? C35A C34A C33A 119.1(5) . . ? C35A C34A H34A 120.4 . . ? C33A C34A H34A 120.4 . . ? C34A C35A C36A 120.2(5) . . ? C34A C35A H35A 119.9 . . ? C36A C35A H35A 119.9 . . ? N31A C36A C35A 121.2(4) . . ? N31A C36A C43A 117.7(4) . . ? C35A C36A C43A 121.1(4) . . ? C45A N41A N42A 111.9(4) . . ? C45A N41A C46A 127.7(4) . . ? N42A N41A C46A 120.3(4) . . ? C43A N42A N41A 104.9(3) . . ? C43A N42A Ag2 114.9(3) . . ? N41A N42A Ag2 140.2(3) . . ? N42A C43A C44A 111.1(4) . . ? N42A C43A C36A 119.2(4) . . ? C44A C43A C36A 129.7(4) . . ? C45A C44A C43A 105.3(4) . . ? C45A C44A H44A 127.4 . . ? C43A C44A H44A 127.4 . . ? N41A C45A C44A 106.8(5) . . ? N41A C45A H45A 126.6 . . ? C44A C45A H45A 126.6 . . ? N41A C46A C54A 115.9(4) . . ? N41A C46A H46A 108.3 . . ? C54A C46A H46A 108.3 . . ? N41A C46A H46B 108.3 . . ? C54A C46A H46B 108.3 . . ? H46A C46A H46B 107.4 . . ? C52A C51A C26A 126.7(4) . . ? C52A C51A S55A 110.5(3) . . ? C26A C51A S55A 122.8(3) . . ? C51A C52A C53A 112.9(4) . . ? C51A C52A H52A 123.5 . . ? C53A C52A H52A 123.5 . . ? C54A C53A C52A 113.0(4) . . ? C54A C53A H53A 123.5 . . ? C52A C53A H53A 123.5 . . ? C53A C54A C46A 125.9(4) . . ? C53A C54A S55A 111.0(3) . . ? C46A C54A S55A 122.9(3) . . ? C54A S55A C51A 92.6(2) . . ? C12B N11B C16B 117.8(4) . . ? C12B N11B Ag1 123.3(3) . . ? C16B N11B Ag1 116.0(3) . . ? N11B C12B C13B 123.8(4) . . ? N11B C12B H12B 118.1 . . ? C13B C12B H12B 118.1 . . ? C12B C13B C14B 118.6(4) . . ? C12B C13B H13B 120.7 . . ? C14B C13B H13B 120.7 . . ? C13B C14B C15B 119.5(5) . . ? C13B C14B H14B 120.3 . . ? C15B C14B H14B 120.3 . . ? C14B C15B C16B 118.8(5) . . ? C14B C15B H15B 120.6 . . ? C16B C15B H15B 120.6 . . ? N11B C16B C15B 121.5(4) . . ? N11B C16B C23B 117.6(4) . . ? C15B C16B C23B 120.9(4) . . ? C25B N21B N22B 111.6(4) . . ? C25B N21B C26B 127.8(4) . . ? N22B N21B C26B 120.5(4) . . ? C23B N22B N21B 105.3(3) . . ? C23B N22B Ag1 112.4(3) . . ? N21B N22B Ag1 142.2(3) . . ? N22B C23B C24B 110.5(4) . . ? N22B C23B C16B 119.1(4) . . ? C24B C23B C16B 130.3(4) . . ? C25B C24B C23B 105.1(4) . . ? C25B C24B H24B 127.4 . . ? C23B C24B H24B 127.4 . . ? N21B C25B C24B 107.4(4) . . ? N21B C25B H25B 126.3 . . ? C24B C25B H25B 126.3 . . ? N21B C26B C51B 115.9(4) . . ? N21B C26B H26C 108.3 . . ? C51B C26B H26C 108.3 . . ? N21B C26B H26D 108.3 . . ? C51B C26B H26D 108.3 . . ? H26C C26B H26D 107.4 . . ? C32B N31B C36B 117.6(4) . . ? C32B N31B Ag2 124.8(3) . . ? C36B N31B Ag2 116.7(3) . . ? N31B C32B C33B 124.3(5) . . ? N31B C32B H32B 117.8 . . ? C33B C32B H32B 117.8 . . ? C34B C33B C32B 117.4(5) . . ? C34B C33B H33B 121.3 . . ? C32B C33B H33B 121.3 . . ? C35B C34B C33B 119.9(5) . . ? C35B C34B H34B 120.0 . . ? C33B C34B H34B 120.0 . . ? C34B C35B C36B 119.2(5) . . ? C34B C35B H35B 120.4 . . ? C36B C35B H35B 120.4 . . ? N31B C36B C35B 121.5(4) . . ? N31B C36B C43B 116.8(4) . . ? C35B C36B C43B 121.8(4) . . ? C45B N41B N42B 112.1(4) . . ? C45B N41B C46B 128.5(4) . . ? N42B N41B C46B 119.3(4) . . ? C43B N42B N41B 105.0(4) . . ? C43B N42B Ag2 113.6(3) . . ? N41B N42B Ag2 141.1(3) . . ? N42B C43B C44B 111.7(4) . . ? N42B C43B C36B 119.9(4) . . ? C44B C43B C36B 128.4(4) . . ? C45B C44B C43B 104.0(5) . . ? C45B C44B H44B 128.0 . . ? C43B C44B H44B 128.0 . . ? N41B C45B C44B 107.1(5) . . ? N41B C45B H45B 126.4 . . ? C44B C45B H45B 126.4 . . ? N41B C46B C54B 115.7(4) . . ? N41B C46B H46C 108.4 . . ? C54B C46B H46C 108.4 . . ? N41B C46B H46D 108.4 . . ? C54B C46B H46D 108.4 . . ? H46C C46B H46D 107.4 . . ? C52B C51B C26B 125.0(5) . . ? C52B C51B S55B 111.6(4) . . ? C26B C51B S55B 123.3(4) . . ? C51B C52B C53B 113.3(5) . . ? C51B C52B H52B 123.4 . . ? C53B C52B H52B 123.4 . . ? C54B C53B C52B 113.2(4) . . ? C54B C53B H53B 123.4 . . ? C52B C53B H53B 123.4 . . ? C53B C54B C46B 125.5(4) . . ? C53B C54B S55B 109.7(4) . . ? C46B C54B S55B 124.8(4) . . ? C51B S55B C54B 92.2(2) . . ? O14Y Cl11 O15X 92.3(5) . . ? O14Y Cl11 O15Y 109.8(5) . . ? O15X Cl11 O15Y 17.7(5) . . ? O14Y Cl11 O13X 122.8(6) . . ? O15X Cl11 O13X 109.4(6) . . ? O15Y Cl11 O13X 100.1(6) . . ? O14Y Cl11 O12X 110.9(6) . . ? O15X Cl11 O12X 107.7(6) . . ? O15Y Cl11 O12X 98.5(6) . . ? O13X Cl11 O12X 111.3(7) . . ? O14Y Cl11 O13Y 112.4(6) . . ? O15X Cl11 O13Y 119.1(6) . . ? O15Y Cl11 O13Y 111.7(6) . . ? O13X Cl11 O13Y 12.6(6) . . ? O12X Cl11 O13Y 112.8(7) . . ? O14Y Cl11 O12Y 107.6(5) . . ? O15X Cl11 O12Y 118.6(6) . . ? O15Y Cl11 O12Y 109.4(5) . . ? O13X Cl11 O12Y 106.6(6) . . ? O12X Cl11 O12Y 11.0(7) . . ? O13Y Cl11 O12Y 105.8(6) . . ? O14Y Cl11 O14X 18.3(5) . . ? O15X Cl11 O14X 108.8(5) . . ? O15Y Cl11 O14X 126.4(5) . . ? O13X Cl11 O14X 108.3(5) . . ? O12X Cl11 O14X 111.3(6) . . ? O13Y Cl11 O14X 96.7(5) . . ? O12Y Cl11 O14X 104.7(4) . . ? O22X Cl21 O23X 88.1(12) . . ? O22X Cl21 O25X 104.9(8) . . ? O23X Cl21 O25X 116.1(5) . . ? O22X Cl21 O22Y 19.1(9) . . ? O23X Cl21 O22Y 106.6(7) . . ? O25X Cl21 O22Y 92.3(6) . . ? O22X Cl21 O24Y 121.9(8) . . ? O23X Cl21 O24Y 110.8(7) . . ? O25X Cl21 O24Y 113.1(5) . . ? O22Y Cl21 O24Y 116.7(6) . . ? O22X Cl21 O24X 102.8(8) . . ? O23X Cl21 O24X 123.3(6) . . ? O25X Cl21 O24X 114.1(5) . . ? O22Y Cl21 O24X 95.6(6) . . ? O24Y Cl21 O24X 21.4(3) . . ? O22X Cl21 O23Y 106.8(15) . . ? O23X Cl21 O23Y 19.2(6) . . ? O25X Cl21 O23Y 113.8(8) . . ? O22Y Cl21 O23Y 125.6(10) . . ? O24Y Cl21 O23Y 96.3(10) . . ? O24X Cl21 O23Y 113.1(9) . . ? O22X Cl21 O25Y 122.8(8) . . ? O23X Cl21 O25Y 107.8(5) . . ? O25X Cl21 O25Y 18.9(4) . . ? O22Y Cl21 O25Y 111.2(6) . . ? O24Y Cl21 O25Y 103.5(6) . . ? O24X Cl21 O25Y 111.4(5) . . ? O23Y Cl21 O25Y 100.2(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11B Ag1 N11A C12A -113.8(7) . . . . ? N22B Ag1 N11A C12A 76.0(4) . . . . ? N22A Ag1 N11A C12A 174.4(4) . . . . ? N11B Ag1 N11A C16A 82.5(7) . . . . ? N22B Ag1 N11A C16A -87.7(3) . . . . ? N22A Ag1 N11A C16A 10.7(3) . . . . ? C16A N11A C12A C13A 0.5(6) . . . . ? Ag1 N11A C12A C13A -162.9(3) . . . . ? N11A C12A C13A C14A -0.5(7) . . . . ? C12A C13A C14A C15A 0.3(7) . . . . ? C13A C14A C15A C16A -0.2(7) . . . . ? C12A N11A C16A C15A -0.5(6) . . . . ? Ag1 N11A C16A C15A 164.0(3) . . . . ? C12A N11A C16A C23A -178.7(4) . . . . ? Ag1 N11A C16A C23A -14.2(5) . . . . ? C14A C15A C16A N11A 0.3(6) . . . . ? C14A C15A C16A C23A 178.6(4) . . . . ? C25A N21A N22A C23A -0.2(4) . . . . ? C26A N21A N22A C23A -178.2(4) . . . . ? C25A N21A N22A Ag1 177.1(4) . . . . ? C26A N21A N22A Ag1 -0.9(7) . . . . ? N11A Ag1 N22A N21A 176.7(5) . . . . ? N11B Ag1 N22A N21A 7.8(5) . . . . ? N22B Ag1 N22A N21A -67.5(5) . . . . ? N11A Ag1 N22A C23A -6.1(3) . . . . ? N11B Ag1 N22A C23A -175.0(3) . . . . ? N22B Ag1 N22A C23A 109.7(3) . . . . ? N21A N22A C23A C24A -0.4(4) . . . . ? Ag1 N22A C23A C24A -178.8(3) . . . . ? N21A N22A C23A C16A 179.7(4) . . . . ? Ag1 N22A C23A C16A 1.3(4) . . . . ? N11A C16A C23A N22A 8.3(6) . . . . ? C15A C16A C23A N22A -170.0(4) . . . . ? N11A C16A C23A C24A -171.6(4) . . . . ? C15A C16A C23A C24A 10.1(7) . . . . ? N22A C23A C24A C25A 0.8(5) . . . . ? C16A C23A C24A C25A -179.3(4) . . . . ? N22A N21A C25A C24A 0.6(5) . . . . ? C26A N21A C25A C24A 178.6(4) . . . . ? C23A C24A C25A N21A -0.8(5) . . . . ? N22A N21A C26A C51A 99.7(5) . . . . ? C25A N21A C26A C51A -78.1(5) . . . . ? N31B Ag2 N31A C32A -36.6(7) . . . . ? N42A Ag2 N31A C32A 178.8(4) . . . . ? N42B Ag2 N31A C32A 71.2(4) . . . . ? N31B Ag2 N31A C36A 154.2(4) . . . . ? N42A Ag2 N31A C36A 9.7(3) . . . . ? N42B Ag2 N31A C36A -98.0(3) . . . . ? C36A N31A C32A C33A 2.2(7) . . . . ? Ag2 N31A C32A C33A -166.6(4) . . . . ? N31A C32A C33A C34A -0.9(8) . . . . ? C32A C33A C34A C35A -0.8(8) . . . . ? C33A C34A C35A C36A 1.0(8) . . . . ? C32A N31A C36A C35A -2.0(6) . . . . ? Ag2 N31A C36A C35A 168.0(3) . . . . ? C32A N31A C36A C43A 177.7(4) . . . . ? Ag2 N31A C36A C43A -12.3(5) . . . . ? C34A C35A C36A N31A 0.4(7) . . . . ? C34A C35A C36A C43A -179.3(4) . . . . ? C45A N41A N42A C43A 0.8(5) . . . . ? C46A N41A N42A C43A 176.7(4) . . . . ? C45A N41A N42A Ag2 177.3(3) . . . . ? C46A N41A N42A Ag2 -6.8(6) . . . . ? N31B Ag2 N42A C43A -175.6(3) . . . . ? N31A Ag2 N42A C43A -6.1(3) . . . . ? N42B Ag2 N42A C43A 102.7(3) . . . . ? N31B Ag2 N42A N41A 8.2(5) . . . . ? N31A Ag2 N42A N41A 177.7(5) . . . . ? N42B Ag2 N42A N41A -73.6(5) . . . . ? N41A N42A C43A C44A -0.1(5) . . . . ? Ag2 N42A C43A C44A -177.6(3) . . . . ? N41A N42A C43A C36A 179.7(4) . . . . ? Ag2 N42A C43A C36A 2.2(5) . . . . ? N31A C36A C43A N42A 6.9(6) . . . . ? C35A C36A C43A N42A -173.4(4) . . . . ? N31A C36A C43A C44A -173.4(4) . . . . ? C35A C36A C43A C44A 6.3(7) . . . . ? N42A C43A C44A C45A -0.6(5) . . . . ? C36A C43A C44A C45A 179.6(4) . . . . ? N42A N41A C45A C44A -1.2(5) . . . . ? C46A N41A C45A C44A -176.8(4) . . . . ? C43A C44A C45A N41A 1.1(5) . . . . ? C45A N41A C46A C54A -111.7(5) . . . . ? N42A N41A C46A C54A 73.0(5) . . . . ? N21A C26A C51A C52A 98.0(5) . . . . ? N21A C26A C51A S55A -83.0(5) . . . . ? C26A C51A C52A C53A 177.7(4) . . . . ? S55A C51A C52A C53A -1.4(5) . . . . ? C51A C52A C53A C54A 1.3(6) . . . . ? C52A C53A C54A C46A -174.5(4) . . . . ? C52A C53A C54A S55A -0.6(5) . . . . ? N41A C46A C54A C53A -127.6(5) . . . . ? N41A C46A C54A S55A 59.2(5) . . . . ? C53A C54A S55A C51A -0.2(4) . . . . ? C46A C54A S55A C51A 173.9(4) . . . . ? C52A C51A S55A C54A 1.0(4) . . . . ? C26A C51A S55A C54A -178.2(4) . . . . ? N11A Ag1 N11B C12B -0.6(8) . . . . ? N22B Ag1 N11B C12B 170.4(4) . . . . ? N22A Ag1 N11B C12B 68.5(3) . . . . ? N11A Ag1 N11B C16B -160.7(5) . . . . ? N22B Ag1 N11B C16B 10.3(3) . . . . ? N22A Ag1 N11B C16B -91.7(3) . . . . ? C16B N11B C12B C13B -0.3(7) . . . . ? Ag1 N11B C12B C13B -160.1(4) . . . . ? N11B C12B C13B C14B 1.7(7) . . . . ? C12B C13B C14B C15B -1.7(7) . . . . ? C13B C14B C15B C16B 0.4(7) . . . . ? C12B N11B C16B C15B -1.0(6) . . . . ? Ag1 N11B C16B C15B 160.2(3) . . . . ? C12B N11B C16B C23B -178.1(4) . . . . ? Ag1 N11B C16B C23B -16.8(5) . . . . ? C14B C15B C16B N11B 1.0(7) . . . . ? C14B C15B C16B C23B 177.9(4) . . . . ? C25B N21B N22B C23B 0.2(5) . . . . ? C26B N21B N22B C23B -178.7(4) . . . . ? C25B N21B N22B Ag1 -175.9(4) . . . . ? C26B N21B N22B Ag1 5.2(7) . . . . ? N11A Ag1 N22B C23B 175.5(3) . . . . ? N11B Ag1 N22B C23B -2.5(3) . . . . ? N22A Ag1 N22B C23B 96.4(3) . . . . ? N11A Ag1 N22B N21B -8.6(5) . . . . ? N11B Ag1 N22B N21B 173.5(5) . . . . ? N22A Ag1 N22B N21B -87.7(5) . . . . ? N21B N22B C23B C24B -0.2(5) . . . . ? Ag1 N22B C23B C24B 177.2(3) . . . . ? N21B N22B C23B C16B 177.5(4) . . . . ? Ag1 N22B C23B C16B -5.1(5) . . . . ? N11B C16B C23B N22B 14.9(6) . . . . ? C15B C16B C23B N22B -162.2(4) . . . . ? N11B C16B C23B C24B -168.0(4) . . . . ? C15B C16B C23B C24B 14.9(7) . . . . ? N22B C23B C24B C25B 0.1(5) . . . . ? C16B C23B C24B C25B -177.2(4) . . . . ? N22B N21B C25B C24B -0.1(5) . . . . ? C26B N21B C25B C24B 178.7(4) . . . . ? C23B C24B C25B N21B 0.0(5) . . . . ? C25B N21B C26B C51B -109.9(5) . . . . ? N22B N21B C26B C51B 68.8(5) . . . . ? N31A Ag2 N31B C32B -67.4(7) . . . . ? N42A Ag2 N31B C32B 72.8(4) . . . . ? N42B Ag2 N31B C32B 179.1(4) . . . . ? N31A Ag2 N31B C36B 123.3(5) . . . . ? N42A Ag2 N31B C36B -96.5(3) . . . . ? N42B Ag2 N31B C36B 9.8(3) . . . . ? C36B N31B C32B C33B 2.0(7) . . . . ? Ag2 N31B C32B C33B -167.2(4) . . . . ? N31B C32B C33B C34B -1.9(8) . . . . ? C32B C33B C34B C35B 0.6(7) . . . . ? C33B C34B C35B C36B 0.3(7) . . . . ? C32B N31B C36B C35B -0.9(6) . . . . ? Ag2 N31B C36B C35B 169.2(3) . . . . ? C32B N31B C36B C43B 178.9(4) . . . . ? Ag2 N31B C36B C43B -11.0(5) . . . . ? C34B C35B C36B N31B -0.2(7) . . . . ? C34B C35B C36B C43B 179.9(4) . . . . ? C45B N41B N42B C43B 1.0(5) . . . . ? C46B N41B N42B C43B 178.6(4) . . . . ? C45B N41B N42B Ag2 173.3(4) . . . . ? C46B N41B N42B Ag2 -9.1(7) . . . . ? N31B Ag2 N42B C43B -7.6(3) . . . . ? N31A Ag2 N42B C43B -171.9(3) . . . . ? N42A Ag2 N42B C43B 108.7(3) . . . . ? N31B Ag2 N42B N41B -179.5(5) . . . . ? N31A Ag2 N42B N41B 16.2(5) . . . . ? N42A Ag2 N42B N41B -63.2(5) . . . . ? N41B N42B C43B C44B -0.3(5) . . . . ? Ag2 N42B C43B C44B -175.1(3) . . . . ? N41B N42B C43B C36B 179.8(4) . . . . ? Ag2 N42B C43B C36B 5.0(5) . . . . ? N31B C36B C43B N42B 3.8(6) . . . . ? C35B C36B C43B N42B -176.4(4) . . . . ? N31B C36B C43B C44B -176.1(4) . . . . ? C35B C36B C43B C44B 3.7(7) . . . . ? N42B C43B C44B C45B -0.4(5) . . . . ? C36B C43B C44B C45B 179.5(5) . . . . ? N42B N41B C45B C44B -1.2(6) . . . . ? C46B N41B C45B C44B -178.5(4) . . . . ? C43B C44B C45B N41B 0.9(5) . . . . ? C45B N41B C46B C54B -81.8(6) . . . . ? N42B N41B C46B C54B 101.1(5) . . . . ? N21B C26B C51B C52B -129.5(5) . . . . ? N21B C26B C51B S55B 54.0(5) . . . . ? C26B C51B C52B C53B -176.2(4) . . . . ? S55B C51B C52B C53B 0.6(5) . . . . ? C51B C52B C53B C54B 0.8(6) . . . . ? C52B C53B C54B C46B 176.3(5) . . . . ? C52B C53B C54B S55B -1.7(5) . . . . ? N41B C46B C54B C53B 104.4(6) . . . . ? N41B C46B C54B S55B -77.8(6) . . . . ? C52B C51B S55B C54B -1.4(4) . . . . ? C26B C51B S55B C54B 175.5(4) . . . . ? C53B C54B S55B C51B 1.8(4) . . . . ? C46B C54B S55B C51B -176.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.336 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.089 data_imw1291p21c _database_code_depnum_ccdc_archive 'CCDC 895600' #TrackingRef 'Ag_Ward_Stephenson_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H44 Ag2 N12, 2(Cl O4)' _chemical_formula_sum 'C56 H44 Ag2 Cl2 N12 O8' _chemical_formula_weight 1299.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6463(10) _cell_length_b 24.0292(15) _cell_length_c 14.4368(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.090(3) _cell_angle_gamma 90.00 _cell_volume 5240.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9880 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7700 _exptl_absorpt_correction_T_max 0.8375 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 98700 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.14 _reflns_number_total 12480 _reflns_number_gt 9592 _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 ; The structure is a [Ag2(L)2](ClO4)2 double helicate. The structure was solved by direct methods and all hydrogens were added in calculated positions. Both ClO4 anions were disordered: The first was completely disordered Cl1X > O15X and Cl1Y > O15Y (57:43), the second was disordered along the Cl21 - O22 bond such that the other three chlorines sat in two positions (60:40). These anions benefitted from global restraints to improve their parameters and bond lengths. 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^)+(0.0483P)^2^+5.0716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12480 _refine_ls_number_parameters 795 _refine_ls_number_restraints 301 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.030324(18) 0.354388(11) 0.614774(17) 0.04298(8) Uani 1 1 d . . . Ag2 Ag 0.50955(2) 0.464135(12) 0.78303(2) 0.05404(10) Uani 1 1 d . . . N11A N 0.01266(18) 0.32290(11) 0.45718(19) 0.0376(6) Uani 1 1 d . . . C12A C -0.0238(2) 0.27440(15) 0.4226(3) 0.0461(8) Uani 1 1 d . . . H12A H -0.0463 0.2509 0.4636 0.055 Uiso 1 1 calc R . . C13A C -0.0304(2) 0.25677(16) 0.3297(3) 0.0530(10) Uani 1 1 d . . . H13A H -0.0580 0.2223 0.3074 0.064 Uiso 1 1 calc R . . C14A C 0.0033(2) 0.28952(16) 0.2710(3) 0.0504(9) Uani 1 1 d . . . H14A H -0.0003 0.2781 0.2071 0.060 Uiso 1 1 calc R . . C15A C 0.0426(2) 0.33950(15) 0.3049(2) 0.0429(8) Uani 1 1 d . . . H15A H 0.0676 0.3626 0.2654 0.052 Uiso 1 1 calc R . . C16A C 0.0449(2) 0.35530(13) 0.3984(2) 0.0333(6) Uani 1 1 d . . . N21A N 0.10841(16) 0.47742(10) 0.53489(17) 0.0303(5) Uani 1 1 d . . . N22A N 0.06996(16) 0.42702(10) 0.52039(17) 0.0306(5) Uani 1 1 d . . . C23A C 0.08144(19) 0.40968(12) 0.4364(2) 0.0304(6) Uani 1 1 d . . . C24A C 0.1264(2) 0.44959(14) 0.3967(2) 0.0384(7) Uani 1 1 d . . . H24A H 0.1421 0.4476 0.3375 0.046 Uiso 1 1 calc R . . C25A C 0.1429(2) 0.49229(13) 0.4623(2) 0.0364(7) Uani 1 1 d . . . H25A H 0.1730 0.5260 0.4573 0.044 Uiso 1 1 calc R . . C26A C 0.1090(2) 0.50807(12) 0.6218(2) 0.0340(6) Uani 1 1 d . . . H26A H 0.0491 0.5063 0.6326 0.041 Uiso 1 1 calc R . . H26B H 0.1222 0.5476 0.6123 0.041 Uiso 1 1 calc R . . N31A N 0.62351(18) 0.40201(11) 0.81617(18) 0.0366(6) Uani 1 1 d . . . C32A C 0.6911(2) 0.40187(15) 0.7752(2) 0.0436(8) Uani 1 1 d . . . H32A H 0.6955 0.4316 0.7334 0.052 Uiso 1 1 calc R . . C33A C 0.7544(3) 0.36088(16) 0.7908(3) 0.0507(9) Uani 1 1 d . . . H33A H 0.8002 0.3617 0.7587 0.061 Uiso 1 1 calc R . . C34A C 0.7502(3) 0.31856(16) 0.8537(3) 0.0510(9) Uani 1 1 d . . . H34A H 0.7938 0.2901 0.8667 0.061 Uiso 1 1 calc R . . C35A C 0.6820(2) 0.31815(14) 0.8974(3) 0.0441(8) Uani 1 1 d . . . H35A H 0.6782 0.2896 0.9416 0.053 Uiso 1 1 calc R . . C36A C 0.6185(2) 0.35995(12) 0.8762(2) 0.0347(6) Uani 1 1 d . . . N41A N 0.42911(18) 0.39118(13) 0.95635(19) 0.0414(6) Uani 1 1 d . . . N42A N 0.49338(17) 0.40515(11) 0.91369(18) 0.0375(6) Uani 1 1 d . . . C43A C 0.5424(2) 0.35943(13) 0.9178(2) 0.0355(7) Uani 1 1 d . . . C44A C 0.5102(3) 0.31675(15) 0.9648(3) 0.0477(8) Uani 1 1 d . . . H44A H 0.5334 0.2802 0.9774 0.057 Uiso 1 1 calc R . . C45A C 0.4387(3) 0.33848(17) 0.9887(3) 0.0506(9) Uani 1 1 d . . . H45A H 0.4021 0.3199 1.0220 0.061 Uiso 1 1 calc R . . C46A C 0.3665(2) 0.43305(17) 0.9696(2) 0.0472(9) Uani 1 1 d . . . H46C H 0.3998 0.4666 0.9983 0.057 Uiso 1 1 calc R . . H46D H 0.3349 0.4187 1.0157 0.057 Uiso 1 1 calc R . . C51A C 0.17512(19) 0.48675(12) 0.7102(2) 0.0289(6) Uani 1 1 d . . . C52A C 0.23249(19) 0.44415(12) 0.7075(2) 0.0311(6) Uani 1 1 d . . . H52A H 0.2305 0.4266 0.6480 0.037 Uiso 1 1 calc R . . C53A C 0.2944(2) 0.42578(12) 0.7912(2) 0.0333(6) Uani 1 1 d . . . H53A H 0.3337 0.3963 0.7872 0.040 Uiso 1 1 calc R . . C54A C 0.2989(2) 0.44980(13) 0.8782(2) 0.0336(6) Uani 1 1 d . . . C55A C 0.2396(2) 0.49363(13) 0.8848(2) 0.0333(6) Uani 1 1 d . . . C56A C 0.17743(19) 0.51259(12) 0.7997(2) 0.0313(6) Uani 1 1 d . . . C61A C 0.2404(2) 0.52006(15) 0.9729(2) 0.0434(8) Uani 1 1 d . . . H61A H 0.2810 0.5078 1.0302 0.052 Uiso 1 1 calc R . . C62A C 0.1841(3) 0.56276(17) 0.9768(2) 0.0519(9) Uani 1 1 d . . . H62A H 0.1856 0.5796 1.0368 0.062 Uiso 1 1 calc R . . C63A C 0.1242(3) 0.58208(17) 0.8934(3) 0.0544(10) Uani 1 1 d . . . H63A H 0.0860 0.6124 0.8966 0.065 Uiso 1 1 calc R . . C64A C 0.1206(2) 0.55716(14) 0.8070(2) 0.0430(8) Uani 1 1 d . . . H64A H 0.0790 0.5701 0.7509 0.052 Uiso 1 1 calc R . . N11B N 0.01894(17) 0.38870(10) 0.76178(18) 0.0332(5) Uani 1 1 d . . . C12B C -0.0387(2) 0.42805(14) 0.7716(2) 0.0423(7) Uani 1 1 d . . . H12B H -0.0821 0.4399 0.7160 0.051 Uiso 1 1 calc R . . C13B C -0.0383(3) 0.45218(15) 0.8582(3) 0.0510(9) Uani 1 1 d . . . H13B H -0.0805 0.4799 0.8622 0.061 Uiso 1 1 calc R . . C14B C 0.0247(3) 0.43514(17) 0.9389(3) 0.0553(10) Uani 1 1 d . . . H14B H 0.0265 0.4508 0.9997 0.066 Uiso 1 1 calc R . . C15B C 0.0850(2) 0.39522(15) 0.9302(2) 0.0442(8) Uani 1 1 d . . . H15B H 0.1294 0.3833 0.9848 0.053 Uiso 1 1 calc R . . C16B C 0.0803(2) 0.37252(12) 0.8407(2) 0.0312(6) Uani 1 1 d . . . N21B N 0.20212(17) 0.27070(10) 0.75314(19) 0.0358(6) Uani 1 1 d . . . N22B N 0.14165(16) 0.31187(10) 0.74006(18) 0.0316(5) Uani 1 1 d . . . C23B C 0.14213(19) 0.32898(12) 0.8286(2) 0.0315(6) Uani 1 1 d . . . C24B C 0.2030(2) 0.29844(16) 0.8978(3) 0.0465(8) Uani 1 1 d . . . H24B H 0.2163 0.3023 0.9655 0.056 Uiso 1 1 calc R . . C25B C 0.2395(2) 0.26167(16) 0.8467(3) 0.0497(9) Uani 1 1 d . . . H25B H 0.2834 0.2346 0.8727 0.060 Uiso 1 1 calc R . . C26B C 0.2218(2) 0.24489(13) 0.6693(3) 0.0385(7) Uani 1 1 d . . . H26C H 0.1662 0.2409 0.6179 0.046 Uiso 1 1 calc R . . H26D H 0.2460 0.2071 0.6867 0.046 Uiso 1 1 calc R . . N31B N 0.42440(18) 0.54220(11) 0.76391(19) 0.0394(6) Uani 1 1 d . . . C32B C 0.4075(3) 0.57199(15) 0.8354(2) 0.0475(8) Uani 1 1 d . . . H32B H 0.4403 0.5635 0.8990 0.057 Uiso 1 1 calc R . . C33B C 0.3462(3) 0.61392(15) 0.8230(3) 0.0498(9) Uani 1 1 d . . . H33B H 0.3364 0.6335 0.8765 0.060 Uiso 1 1 calc R . . C34B C 0.2992(2) 0.62676(14) 0.7314(3) 0.0453(8) Uani 1 1 d . . . H34B H 0.2566 0.6558 0.7201 0.054 Uiso 1 1 calc R . . C35B C 0.3146(2) 0.59685(13) 0.6558(2) 0.0401(7) Uani 1 1 d . . . H35B H 0.2830 0.6053 0.5918 0.048 Uiso 1 1 calc R . . C36B C 0.3768(2) 0.55420(12) 0.6739(2) 0.0331(6) Uani 1 1 d . . . N41B N 0.42773(18) 0.44659(11) 0.53063(19) 0.0370(6) Uani 1 1 d . . . N42B N 0.42872(17) 0.46916(10) 0.61654(19) 0.0352(6) Uani 1 1 d . . . C43B C 0.3901(2) 0.51897(12) 0.5960(2) 0.0319(6) Uani 1 1 d . . . C44B C 0.3639(2) 0.52760(13) 0.4964(2) 0.0362(7) Uani 1 1 d . . . H44B H 0.3350 0.5593 0.4632 0.043 Uiso 1 1 calc R . . C45B C 0.3890(2) 0.48038(14) 0.4576(2) 0.0396(7) Uani 1 1 d . . . H45B H 0.3805 0.4728 0.3912 0.048 Uiso 1 1 calc R . . C46B C 0.4597(2) 0.38998(14) 0.5272(3) 0.0470(8) Uani 1 1 d . . . H46A H 0.5210 0.3871 0.5683 0.056 Uiso 1 1 calc R . . H46B H 0.4605 0.3808 0.4606 0.056 Uiso 1 1 calc R . . C51B C 0.2873(2) 0.27826(11) 0.6315(2) 0.0314(6) Uani 1 1 d . . . C52B C 0.2549(2) 0.31996(12) 0.5666(2) 0.0345(6) Uani 1 1 d . . . H52B H 0.1927 0.3251 0.5442 0.041 Uiso 1 1 calc R . . C53B C 0.3116(2) 0.35496(13) 0.5328(2) 0.0373(7) Uani 1 1 d . . . H53B H 0.2872 0.3838 0.4888 0.045 Uiso 1 1 calc R . . C54B C 0.4008(2) 0.34853(12) 0.5617(2) 0.0347(6) Uani 1 1 d . . . C55B C 0.4377(2) 0.30374(12) 0.6238(2) 0.0320(6) Uani 1 1 d . . . C56B C 0.3800(2) 0.26878(12) 0.6610(2) 0.0323(6) Uani 1 1 d . . . C61B C 0.5294(2) 0.29158(13) 0.6501(3) 0.0408(7) Uani 1 1 d . . . H61B H 0.5686 0.3142 0.6261 0.049 Uiso 1 1 calc R . . C62B C 0.5626(2) 0.24815(15) 0.7092(3) 0.0504(9) Uani 1 1 d . . . H62B H 0.6242 0.2402 0.7246 0.060 Uiso 1 1 calc R . . C63B C 0.5064(3) 0.21517(15) 0.7473(3) 0.0517(9) Uani 1 1 d . . . H63B H 0.5303 0.1855 0.7897 0.062 Uiso 1 1 calc R . . C64B C 0.4182(2) 0.22512(14) 0.7242(3) 0.0431(8) Uani 1 1 d . . . H64B H 0.3811 0.2023 0.7510 0.052 Uiso 1 1 calc R . . Cl1X Cl 0.26174(18) 0.41423(10) 0.2024(2) 0.0441(4) Uani 0.574(5) 1 d PDU A 1 Cl1Y Cl 0.2706(2) 0.41704(14) 0.2061(3) 0.0446(4) Uani 0.426(5) 1 d PDU A 2 O12X O 0.2871(3) 0.3847(2) 0.2920(3) 0.0511(8) Uani 0.574(5) 1 d PDU A 1 O13X O 0.1685(2) 0.4267(2) 0.1794(3) 0.0590(8) Uani 0.574(5) 1 d PDU A 1 O14X O 0.3113(3) 0.46511(14) 0.2097(3) 0.0620(9) Uani 0.574(5) 1 d PDU A 1 O15X O 0.2795(3) 0.38013(18) 0.1274(3) 0.0472(8) Uani 0.574(5) 1 d PDU A 1 O12Y O 0.2745(4) 0.3809(2) 0.2864(5) 0.0501(9) Uani 0.426(5) 1 d PDU A 2 O13Y O 0.2012(4) 0.4574(2) 0.1992(4) 0.0580(9) Uani 0.426(5) 1 d PDU A 2 O14Y O 0.2531(4) 0.3848(3) 0.1192(4) 0.0481(9) Uani 0.426(5) 1 d PDU A 2 O15Y O 0.3540(3) 0.4455(2) 0.2192(4) 0.0557(9) Uani 0.426(5) 1 d PDU A 2 Cl21 Cl 0.79536(6) 0.31354(4) 0.55791(6) 0.0521(2) Uani 1 1 d DU . . O22 O 0.79210(17) 0.30096(10) 0.45968(11) 0.0657(7) Uani 1 1 d DU B . O23X O 0.8790(2) 0.29200(19) 0.6177(2) 0.0690(11) Uani 0.599(7) 1 d PDU B 1 O24X O 0.7242(3) 0.2867(2) 0.5851(3) 0.0741(10) Uani 0.599(7) 1 d PDU B 1 O25X O 0.7933(4) 0.37230(8) 0.5718(2) 0.0605(10) Uani 0.599(7) 1 d PDU B 1 O23Y O 0.8461(5) 0.2736(2) 0.6206(2) 0.0759(13) Uani 0.401(7) 1 d PDU B 2 O24Y O 0.70543(19) 0.3145(3) 0.5675(3) 0.0694(11) Uani 0.401(7) 1 d PDU B 2 O25Y O 0.8326(5) 0.36843(15) 0.5803(3) 0.0587(12) Uani 0.401(7) 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 0.04807(16) 0.05399(16) 0.02779(12) 0.00030(10) 0.01152(10) -0.00342(12) Ag2 0.05405(18) 0.04976(17) 0.05098(17) 0.02199(13) 0.00058(13) 0.00845(13) N11A 0.0341(14) 0.0393(14) 0.0380(14) -0.0087(11) 0.0072(11) -0.0005(11) C12A 0.0370(18) 0.0422(18) 0.058(2) -0.0122(16) 0.0102(15) -0.0041(14) C13A 0.040(2) 0.046(2) 0.067(2) -0.0251(18) 0.0037(17) 0.0001(16) C14A 0.051(2) 0.054(2) 0.0419(19) -0.0204(17) 0.0036(16) 0.0111(17) C15A 0.047(2) 0.0487(19) 0.0310(16) -0.0071(14) 0.0065(14) 0.0123(15) C16A 0.0289(15) 0.0375(15) 0.0303(14) -0.0046(12) 0.0022(12) 0.0081(12) N21A 0.0312(13) 0.0321(12) 0.0257(12) -0.0003(9) 0.0035(10) 0.0002(10) N22A 0.0345(13) 0.0308(12) 0.0257(12) -0.0021(9) 0.0064(10) -0.0004(10) C23A 0.0279(14) 0.0373(15) 0.0252(13) -0.0018(11) 0.0053(11) 0.0061(12) C24A 0.0371(17) 0.0479(18) 0.0318(15) -0.0001(13) 0.0121(13) 0.0033(14) C25A 0.0341(16) 0.0393(16) 0.0352(16) 0.0047(13) 0.0081(13) -0.0019(13) C26A 0.0374(17) 0.0322(15) 0.0292(14) -0.0049(12) 0.0027(12) 0.0039(12) N31A 0.0401(15) 0.0392(14) 0.0287(13) 0.0031(11) 0.0057(11) 0.0007(11) C32A 0.046(2) 0.053(2) 0.0321(16) -0.0009(14) 0.0108(14) -0.0049(16) C33A 0.046(2) 0.061(2) 0.049(2) -0.0146(18) 0.0195(17) -0.0035(17) C34A 0.047(2) 0.046(2) 0.060(2) -0.0077(17) 0.0143(17) 0.0082(16) C35A 0.047(2) 0.0361(17) 0.0487(19) 0.0047(14) 0.0120(16) 0.0054(14) C36A 0.0395(17) 0.0337(15) 0.0287(14) -0.0011(12) 0.0052(12) 0.0009(13) N41A 0.0354(15) 0.0588(17) 0.0295(13) 0.0133(12) 0.0073(11) 0.0074(13) N42A 0.0365(14) 0.0470(15) 0.0297(13) 0.0096(11) 0.0101(11) 0.0070(12) C43A 0.0373(17) 0.0395(16) 0.0265(14) 0.0062(12) 0.0023(12) 0.0039(13) C44A 0.052(2) 0.0433(19) 0.047(2) 0.0136(15) 0.0106(16) 0.0009(16) C45A 0.050(2) 0.062(2) 0.0396(18) 0.0165(17) 0.0109(16) -0.0049(18) C46A 0.0380(18) 0.075(3) 0.0289(16) 0.0074(16) 0.0097(13) 0.0118(17) C51A 0.0300(15) 0.0288(14) 0.0269(14) -0.0009(11) 0.0057(11) -0.0025(11) C52A 0.0327(15) 0.0325(14) 0.0283(14) -0.0043(11) 0.0083(12) -0.0028(12) C53A 0.0320(15) 0.0336(15) 0.0350(15) 0.0026(12) 0.0102(12) 0.0032(12) C54A 0.0296(15) 0.0443(17) 0.0271(14) 0.0047(12) 0.0080(11) -0.0018(12) C55A 0.0332(16) 0.0395(16) 0.0284(14) -0.0043(12) 0.0103(12) -0.0053(12) C56A 0.0311(15) 0.0323(14) 0.0302(14) -0.0047(12) 0.0074(12) -0.0033(12) C61A 0.0427(19) 0.058(2) 0.0291(16) -0.0080(14) 0.0081(13) -0.0035(16) C62A 0.058(2) 0.065(2) 0.0332(17) -0.0193(16) 0.0137(16) 0.0035(19) C63A 0.058(2) 0.056(2) 0.049(2) -0.0167(17) 0.0116(18) 0.0137(18) C64A 0.0466(19) 0.0438(18) 0.0355(17) -0.0086(14) 0.0050(14) 0.0085(15) N11B 0.0368(14) 0.0349(13) 0.0298(13) 0.0016(10) 0.0120(11) 0.0014(11) C12B 0.0445(19) 0.0404(17) 0.0425(18) 0.0024(14) 0.0120(15) 0.0050(14) C13B 0.056(2) 0.0443(19) 0.057(2) -0.0087(17) 0.0220(18) 0.0089(16) C14B 0.066(3) 0.057(2) 0.044(2) -0.0164(17) 0.0184(18) 0.0037(19) C15B 0.049(2) 0.0513(19) 0.0310(16) -0.0055(14) 0.0074(14) 0.0002(16) C16B 0.0333(15) 0.0309(14) 0.0309(14) -0.0001(11) 0.0108(12) -0.0063(12) N21B 0.0371(14) 0.0321(13) 0.0420(14) 0.0072(11) 0.0172(11) 0.0051(11) N22B 0.0332(13) 0.0281(12) 0.0354(13) 0.0030(10) 0.0122(10) 0.0014(10) C23B 0.0298(15) 0.0355(15) 0.0307(14) 0.0030(12) 0.0107(12) -0.0029(12) C24B 0.045(2) 0.058(2) 0.0368(17) 0.0136(16) 0.0126(15) 0.0078(16) C25B 0.048(2) 0.055(2) 0.050(2) 0.0215(17) 0.0191(16) 0.0176(17) C26B 0.0385(17) 0.0289(15) 0.0530(19) -0.0045(13) 0.0206(15) -0.0007(13) N31B 0.0416(15) 0.0377(14) 0.0334(14) 0.0036(11) -0.0002(11) -0.0063(11) C32B 0.058(2) 0.0464(19) 0.0340(17) -0.0003(15) 0.0053(15) -0.0114(17) C33B 0.062(2) 0.0432(19) 0.044(2) -0.0105(15) 0.0143(17) -0.0131(17) C34B 0.049(2) 0.0326(16) 0.054(2) -0.0045(15) 0.0131(16) -0.0035(14) C35B 0.0438(19) 0.0332(15) 0.0390(17) 0.0034(13) 0.0032(14) -0.0037(13) C36B 0.0366(16) 0.0290(14) 0.0318(15) 0.0048(12) 0.0054(12) -0.0098(12) N41B 0.0396(15) 0.0329(13) 0.0409(15) -0.0003(11) 0.0148(12) -0.0057(11) N42B 0.0362(14) 0.0327(13) 0.0358(14) 0.0036(10) 0.0078(11) -0.0026(11) C43B 0.0317(15) 0.0293(14) 0.0327(15) 0.0047(11) 0.0048(12) -0.0061(11) C44B 0.0376(17) 0.0367(16) 0.0328(15) 0.0068(12) 0.0063(13) -0.0046(13) C45B 0.0417(18) 0.0445(18) 0.0324(16) 0.0014(13) 0.0093(13) -0.0088(14) C46B 0.048(2) 0.0361(17) 0.066(2) -0.0011(16) 0.0320(18) -0.0003(15) C51B 0.0347(16) 0.0260(13) 0.0362(15) -0.0065(12) 0.0142(12) -0.0005(11) C52B 0.0300(15) 0.0340(15) 0.0399(16) -0.0025(13) 0.0101(12) 0.0018(12) C53B 0.0401(17) 0.0340(15) 0.0403(17) 0.0032(13) 0.0146(14) 0.0013(13) C54B 0.0362(16) 0.0308(15) 0.0405(16) -0.0073(12) 0.0160(13) -0.0016(12) C55B 0.0313(15) 0.0279(14) 0.0384(16) -0.0091(12) 0.0120(12) 0.0017(11) C56B 0.0357(16) 0.0277(14) 0.0349(15) -0.0056(11) 0.0119(12) 0.0025(12) C61B 0.0320(17) 0.0347(16) 0.057(2) -0.0124(15) 0.0133(14) -0.0024(13) C62B 0.0339(18) 0.0445(19) 0.067(2) -0.0110(17) 0.0025(16) 0.0103(15) C63B 0.052(2) 0.0440(19) 0.055(2) 0.0023(17) 0.0059(17) 0.0156(17) C64B 0.049(2) 0.0353(16) 0.0481(19) 0.0022(14) 0.0181(16) 0.0085(14) Cl1X 0.0677(8) 0.0336(6) 0.0348(6) 0.0026(5) 0.0199(6) 0.0045(6) Cl1Y 0.0664(9) 0.0359(8) 0.0359(8) 0.0024(7) 0.0214(8) 0.0042(7) O12X 0.0769(17) 0.0421(15) 0.0352(13) 0.0037(12) 0.0160(14) 0.0029(14) O13X 0.0713(13) 0.0579(17) 0.0499(16) -0.0014(15) 0.0196(14) 0.0136(14) O14X 0.0856(18) 0.0395(14) 0.0542(16) 0.0047(14) 0.0065(17) -0.0056(14) O15X 0.0649(18) 0.0436(15) 0.0363(13) 0.0007(12) 0.0191(14) 0.0072(15) O12Y 0.0754(18) 0.0410(16) 0.0356(14) 0.0042(13) 0.0178(16) 0.0033(15) O13Y 0.0769(17) 0.0492(17) 0.0514(17) 0.0042(16) 0.0229(16) 0.0163(14) O14Y 0.0664(19) 0.0425(16) 0.0360(14) 0.0001(13) 0.0146(16) 0.0041(16) O15Y 0.0721(16) 0.0432(18) 0.0514(17) 0.0006(16) 0.0153(17) -0.0050(14) Cl21 0.0553(5) 0.0506(5) 0.0462(5) -0.0030(4) 0.0057(4) 0.0021(4) O22 0.0759(17) 0.0658(15) 0.0528(11) -0.0122(12) 0.0122(12) 0.0102(14) O23X 0.0667(17) 0.056(2) 0.0686(18) 0.0190(18) -0.0101(17) -0.0062(17) O24X 0.0702(18) 0.071(2) 0.086(2) -0.011(2) 0.0289(16) -0.0059(17) O25X 0.063(2) 0.0510(12) 0.0536(18) -0.0067(14) -0.0099(18) 0.0087(15) O23Y 0.076(2) 0.062(2) 0.071(2) 0.0122(19) -0.013(2) -0.004(2) O24Y 0.0641(15) 0.070(2) 0.077(2) -0.002(2) 0.0228(17) -0.0010(19) O25Y 0.055(2) 0.0521(15) 0.056(2) -0.0077(17) -0.009(2) 0.0026(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11B 2.326(2) . ? Ag1 N11A 2.345(3) . ? Ag1 N22B 2.389(2) . ? Ag1 N22A 2.393(2) . ? Ag2 N31B 2.276(3) . ? Ag2 N31A 2.279(3) . ? Ag2 N42B 2.410(3) . ? Ag2 N42A 2.425(3) . ? N11A C12A 1.336(4) . ? N11A C16A 1.343(4) . ? C12A C13A 1.383(5) . ? C12A H12A 0.9500 . ? C13A C14A 1.360(6) . ? C13A H13A 0.9500 . ? C14A C15A 1.380(5) . ? C14A H14A 0.9500 . ? C15A C16A 1.394(4) . ? C15A H15A 0.9500 . ? C16A C23A 1.473(4) . ? N21A N22A 1.344(3) . ? N21A C25A 1.346(4) . ? N21A C26A 1.453(4) . ? N22A C23A 1.338(4) . ? C23A C24A 1.397(4) . ? C24A C25A 1.374(5) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C26A C51A 1.508(4) . ? C26A H26A 0.9900 . ? C26A H26B 0.9900 . ? N31A C32A 1.339(4) . ? N31A C36A 1.347(4) . ? C32A C33A 1.373(5) . ? C32A H32A 0.9500 . ? C33A C34A 1.376(6) . ? C33A H33A 0.9500 . ? C34A C35A 1.374(5) . ? C34A H34A 0.9500 . ? C35A C36A 1.390(5) . ? C35A H35A 0.9500 . ? C36A C43A 1.465(5) . ? N41A C45A 1.344(5) . ? N41A N42A 1.351(4) . ? N41A C46A 1.450(4) . ? N42A C43A 1.333(4) . ? C43A C44A 1.394(5) . ? C44A C45A 1.358(5) . ? C44A H44A 0.9500 . ? C45A H45A 0.9500 . ? C46A C54A 1.515(4) . ? C46A H46C 0.9900 . ? C46A H46D 0.9900 . ? C51A C52A 1.369(4) . ? C51A C56A 1.425(4) . ? C52A C53A 1.409(4) . ? C52A H52A 0.9500 . ? C53A C54A 1.367(4) . ? C53A H53A 0.9500 . ? C54A C55A 1.424(4) . ? C55A C61A 1.418(4) . ? C55A C56A 1.429(4) . ? C56A C64A 1.414(4) . ? C61A C62A 1.363(5) . ? C61A H61A 0.9500 . ? C62A C63A 1.399(5) . ? C62A H62A 0.9500 . ? C63A C64A 1.372(5) . ? C63A H63A 0.9500 . ? C64A H64A 0.9500 . ? N11B C12B 1.340(4) . ? N11B C16B 1.342(4) . ? C12B C13B 1.376(5) . ? C12B H12B 0.9500 . ? C13B C14B 1.378(6) . ? C13B H13B 0.9500 . ? C14B C15B 1.374(5) . ? C14B H14B 0.9500 . ? C15B C16B 1.386(4) . ? C15B H15B 0.9500 . ? C16B C23B 1.466(4) . ? N21B C25B 1.342(4) . ? N21B N22B 1.348(3) . ? N21B C26B 1.463(4) . ? N22B C23B 1.341(4) . ? C23B C24B 1.396(4) . ? C24B C25B 1.367(5) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C26B C51B 1.511(4) . ? C26B H26C 0.9900 . ? C26B H26D 0.9900 . ? N31B C32B 1.338(5) . ? N31B C36B 1.350(4) . ? C32B C33B 1.371(5) . ? C32B H32B 0.9500 . ? C33B C34B 1.371(5) . ? C33B H33B 0.9500 . ? C34B C35B 1.380(5) . ? C34B H34B 0.9500 . ? C35B C36B 1.390(5) . ? C35B H35B 0.9500 . ? C36B C43B 1.465(4) . ? N41B C45B 1.344(4) . ? N41B N42B 1.350(4) . ? N41B C46B 1.454(4) . ? N42B C43B 1.339(4) . ? C43B C44B 1.405(4) . ? C44B C45B 1.367(5) . ? C44B H44B 0.9500 . ? C45B H45B 0.9500 . ? C46B C54B 1.525(4) . ? C46B H46A 0.9900 . ? C46B H46B 0.9900 . ? C51B C52B 1.375(4) . ? C51B C56B 1.419(4) . ? C52B C53B 1.399(4) . ? C52B H52B 0.9500 . ? C53B C54B 1.358(5) . ? C53B H53B 0.9500 . ? C54B C55B 1.423(4) . ? C55B C61B 1.416(4) . ? C55B C56B 1.437(4) . ? C56B C64B 1.416(4) . ? C61B C62B 1.362(5) . ? C61B H61B 0.9500 . ? C62B C63B 1.398(6) . ? C62B H62B 0.9500 . ? C63B C64B 1.354(5) . ? C63B H63B 0.9500 . ? C64B H64B 0.9500 . ? Cl1X O12X 1.437(2) . ? Cl1X O14X 1.437(2) . ? Cl1X O13X 1.441(2) . ? Cl1X O15X 1.442(2) . ? Cl1Y O12Y 1.437(2) . ? Cl1Y O14Y 1.439(2) . ? Cl1Y O13Y 1.439(2) . ? Cl1Y O15Y 1.443(2) . ? Cl21 O23Y 1.413(2) . ? Cl21 O24X 1.4270(19) . ? Cl21 O25X 1.4277(19) . ? Cl21 O22 1.4377(13) . ? Cl21 O25Y 1.444(2) . ? Cl21 O24Y 1.449(2) . ? Cl21 O23X 1.4613(19) . ? 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 N11B Ag1 N11A 169.07(9) . . ? N11B Ag1 N22B 71.02(9) . . ? N11A Ag1 N22B 118.37(9) . . ? N11B Ag1 N22A 110.71(8) . . ? N11A Ag1 N22A 70.45(9) . . ? N22B Ag1 N22A 119.80(8) . . ? N31B Ag2 N31A 165.22(10) . . ? N31B Ag2 N42B 72.49(9) . . ? N31A Ag2 N42B 114.89(9) . . ? N31B Ag2 N42A 113.57(10) . . ? N31A Ag2 N42A 71.83(9) . . ? N42B Ag2 N42A 132.16(9) . . ? C12A N11A C16A 117.6(3) . . ? C12A N11A Ag1 125.1(2) . . ? C16A N11A Ag1 117.20(19) . . ? N11A C12A C13A 123.1(4) . . ? N11A C12A H12A 118.4 . . ? C13A C12A H12A 118.4 . . ? C14A C13A C12A 118.9(3) . . ? C14A C13A H13A 120.5 . . ? C12A C13A H13A 120.5 . . ? C13A C14A C15A 119.5(3) . . ? C13A C14A H14A 120.3 . . ? C15A C14A H14A 120.3 . . ? C14A C15A C16A 118.5(3) . . ? C14A C15A H15A 120.7 . . ? C16A C15A H15A 120.7 . . ? N11A C16A C15A 122.3(3) . . ? N11A C16A C23A 116.9(3) . . ? C15A C16A C23A 120.8(3) . . ? N22A N21A C25A 111.8(2) . . ? N22A N21A C26A 119.5(2) . . ? C25A N21A C26A 128.6(3) . . ? C23A N22A N21A 105.2(2) . . ? C23A N22A Ag1 113.87(19) . . ? N21A N22A Ag1 137.75(18) . . ? N22A C23A C24A 111.0(3) . . ? N22A C23A C16A 118.9(3) . . ? C24A C23A C16A 130.1(3) . . ? C25A C24A C23A 104.7(3) . . ? C25A C24A H24A 127.6 . . ? C23A C24A H24A 127.6 . . ? N21A C25A C24A 107.3(3) . . ? N21A C25A H25A 126.4 . . ? C24A C25A H25A 126.4 . . ? N21A C26A C51A 114.0(2) . . ? N21A C26A H26A 108.7 . . ? C51A C26A H26A 108.7 . . ? N21A C26A H26B 108.7 . . ? C51A C26A H26B 108.7 . . ? H26A C26A H26B 107.6 . . ? C32A N31A C36A 117.9(3) . . ? C32A N31A Ag2 125.0(2) . . ? C36A N31A Ag2 116.9(2) . . ? N31A C32A C33A 123.3(3) . . ? N31A C32A H32A 118.4 . . ? C33A C32A H32A 118.4 . . ? C32A C33A C34A 118.8(3) . . ? C32A C33A H33A 120.6 . . ? C34A C33A H33A 120.6 . . ? C35A C34A C33A 119.0(3) . . ? C35A C34A H34A 120.5 . . ? C33A C34A H34A 120.5 . . ? C34A C35A C36A 119.4(3) . . ? C34A C35A H35A 120.3 . . ? C36A C35A H35A 120.3 . . ? N31A C36A C35A 121.7(3) . . ? N31A C36A C43A 117.4(3) . . ? C35A C36A C43A 120.9(3) . . ? C45A N41A N42A 111.3(3) . . ? C45A N41A C46A 128.7(3) . . ? N42A N41A C46A 119.7(3) . . ? C43A N42A N41A 105.3(3) . . ? C43A N42A Ag2 109.9(2) . . ? N41A N42A Ag2 137.78(19) . . ? N42A C43A C44A 110.5(3) . . ? N42A C43A C36A 119.6(3) . . ? C44A C43A C36A 129.8(3) . . ? C45A C44A C43A 105.5(3) . . ? C45A C44A H44A 127.3 . . ? C43A C44A H44A 127.3 . . ? N41A C45A C44A 107.4(3) . . ? N41A C45A H45A 126.3 . . ? C44A C45A H45A 126.3 . . ? N41A C46A C54A 114.3(3) . . ? N41A C46A H46C 108.7 . . ? C54A C46A H46C 108.7 . . ? N41A C46A H46D 108.7 . . ? C54A C46A H46D 108.7 . . ? H46C C46A H46D 107.6 . . ? C52A C51A C56A 119.3(3) . . ? C52A C51A C26A 122.7(3) . . ? C56A C51A C26A 118.0(3) . . ? C51A C52A C53A 121.3(3) . . ? C51A C52A H52A 119.3 . . ? C53A C52A H52A 119.3 . . ? C54A C53A C52A 121.0(3) . . ? C54A C53A H53A 119.5 . . ? C52A C53A H53A 119.5 . . ? C53A C54A C55A 119.7(3) . . ? C53A C54A C46A 123.0(3) . . ? C55A C54A C46A 117.3(3) . . ? C61A C55A C54A 122.5(3) . . ? C61A C55A C56A 118.3(3) . . ? C54A C55A C56A 119.2(3) . . ? C64A C56A C51A 122.0(3) . . ? C64A C56A C55A 118.5(3) . . ? C51A C56A C55A 119.5(3) . . ? C62A C61A C55A 121.3(3) . . ? C62A C61A H61A 119.3 . . ? C55A C61A H61A 119.3 . . ? C61A C62A C63A 120.6(3) . . ? C61A C62A H62A 119.7 . . ? C63A C62A H62A 119.7 . . ? C64A C63A C62A 119.8(3) . . ? C64A C63A H63A 120.1 . . ? C62A C63A H63A 120.1 . . ? C63A C64A C56A 121.4(3) . . ? C63A C64A H64A 119.3 . . ? C56A C64A H64A 119.3 . . ? C12B N11B C16B 117.9(3) . . ? C12B N11B Ag1 124.1(2) . . ? C16B N11B Ag1 117.6(2) . . ? N11B C12B C13B 123.4(3) . . ? N11B C12B H12B 118.3 . . ? C13B C12B H12B 118.3 . . ? C12B C13B C14B 118.4(3) . . ? C12B C13B H13B 120.8 . . ? C14B C13B H13B 120.8 . . ? C15B C14B C13B 119.2(3) . . ? C15B C14B H14B 120.4 . . ? C13B C14B H14B 120.4 . . ? C14B C15B C16B 119.3(3) . . ? C14B C15B H15B 120.4 . . ? C16B C15B H15B 120.4 . . ? N11B C16B C15B 122.0(3) . . ? N11B C16B C23B 117.0(3) . . ? C15B C16B C23B 121.0(3) . . ? C25B N21B N22B 111.5(3) . . ? C25B N21B C26B 129.3(3) . . ? N22B N21B C26B 119.1(3) . . ? C23B N22B N21B 105.2(2) . . ? C23B N22B Ag1 114.37(19) . . ? N21B N22B Ag1 140.1(2) . . ? N22B C23B C24B 110.7(3) . . ? N22B C23B C16B 119.5(3) . . ? C24B C23B C16B 129.8(3) . . ? C25B C24B C23B 104.9(3) . . ? C25B C24B H24B 127.5 . . ? C23B C24B H24B 127.5 . . ? N21B C25B C24B 107.7(3) . . ? N21B C25B H25B 126.1 . . ? C24B C25B H25B 126.1 . . ? N21B C26B C51B 112.5(2) . . ? N21B C26B H26C 109.1 . . ? C51B C26B H26C 109.1 . . ? N21B C26B H26D 109.1 . . ? C51B C26B H26D 109.1 . . ? H26C C26B H26D 107.8 . . ? C32B N31B C36B 117.2(3) . . ? C32B N31B Ag2 125.1(2) . . ? C36B N31B Ag2 116.9(2) . . ? N31B C32B C33B 124.4(3) . . ? N31B C32B H32B 117.8 . . ? C33B C32B H32B 117.8 . . ? C34B C33B C32B 118.2(3) . . ? C34B C33B H33B 120.9 . . ? C32B C33B H33B 120.9 . . ? C33B C34B C35B 119.1(3) . . ? C33B C34B H34B 120.5 . . ? C35B C34B H34B 120.5 . . ? C34B C35B C36B 119.5(3) . . ? C34B C35B H35B 120.2 . . ? C36B C35B H35B 120.2 . . ? N31B C36B C35B 121.5(3) . . ? N31B C36B C43B 117.5(3) . . ? C35B C36B C43B 120.9(3) . . ? C45B N41B N42B 111.9(3) . . ? C45B N41B C46B 128.9(3) . . ? N42B N41B C46B 119.0(3) . . ? C43B N42B N41B 105.0(2) . . ? C43B N42B Ag2 110.77(19) . . ? N41B N42B Ag2 140.7(2) . . ? N42B C43B C44B 110.7(3) . . ? N42B C43B C36B 119.5(3) . . ? C44B C43B C36B 129.7(3) . . ? C45B C44B C43B 105.0(3) . . ? C45B C44B H44B 127.5 . . ? C43B C44B H44B 127.5 . . ? N41B C45B C44B 107.4(3) . . ? N41B C45B H45B 126.3 . . ? C44B C45B H45B 126.3 . . ? N41B C46B C54B 111.0(3) . . ? N41B C46B H46A 109.4 . . ? C54B C46B H46A 109.4 . . ? N41B C46B H46B 109.4 . . ? C54B C46B H46B 109.4 . . ? H46A C46B H46B 108.0 . . ? C52B C51B C56B 119.2(3) . . ? C52B C51B C26B 117.9(3) . . ? C56B C51B C26B 122.9(3) . . ? C51B C52B C53B 121.4(3) . . ? C51B C52B H52B 119.3 . . ? C53B C52B H52B 119.3 . . ? C54B C53B C52B 121.3(3) . . ? C54B C53B H53B 119.4 . . ? C52B C53B H53B 119.4 . . ? C53B C54B C55B 119.7(3) . . ? C53B C54B C46B 119.0(3) . . ? C55B C54B C46B 121.3(3) . . ? C61B C55B C54B 122.8(3) . . ? C61B C55B C56B 118.1(3) . . ? C54B C55B C56B 119.1(3) . . ? C64B C56B C51B 122.7(3) . . ? C64B C56B C55B 118.2(3) . . ? C51B C56B C55B 119.1(3) . . ? C62B C61B C55B 121.4(3) . . ? C62B C61B H61B 119.3 . . ? C55B C61B H61B 119.3 . . ? C61B C62B C63B 120.3(3) . . ? C61B C62B H62B 119.9 . . ? C63B C62B H62B 119.9 . . ? C64B C63B C62B 120.6(3) . . ? C64B C63B H63B 119.7 . . ? C62B C63B H63B 119.7 . . ? C63B C64B C56B 121.4(3) . . ? C63B C64B H64B 119.3 . . ? C56B C64B H64B 119.3 . . ? O12X Cl1X O14X 109.67(14) . . ? O12X Cl1X O13X 109.60(14) . . ? O14X Cl1X O13X 109.53(14) . . ? O12X Cl1X O15X 109.51(14) . . ? O14X Cl1X O15X 109.42(14) . . ? O13X Cl1X O15X 109.10(14) . . ? O12Y Cl1Y O14Y 109.69(15) . . ? O12Y Cl1Y O13Y 109.64(15) . . ? O14Y Cl1Y O13Y 109.50(15) . . ? O12Y Cl1Y O15Y 109.49(15) . . ? O14Y Cl1Y O15Y 109.27(15) . . ? O13Y Cl1Y O15Y 109.22(15) . . ? O23Y Cl21 O24X 82.2(3) . . ? O23Y Cl21 O25X 127.7(2) . . ? O24X Cl21 O25X 111.13(13) . . ? O23Y Cl21 O22 111.03(14) . . ? O24X Cl21 O22 110.28(13) . . ? O25X Cl21 O22 110.49(13) . . ? O23Y Cl21 O25Y 110.51(14) . . ? O24X Cl21 O25Y 130.5(2) . . ? O25X Cl21 O25Y 24.2(2) . . ? O22 Cl21 O25Y 108.77(14) . . ? O23Y Cl21 O24Y 110.30(14) . . ? O24X Cl21 O24Y 30.1(2) . . ? O25X Cl21 O24Y 85.0(2) . . ? O22 Cl21 O24Y 108.12(14) . . ? O25Y Cl21 O24Y 108.03(14) . . ? O23Y Cl21 O23X 27.6(2) . . ? O24X Cl21 O23X 108.64(13) . . ? O25X Cl21 O23X 108.47(13) . . ? O22 Cl21 O23X 107.73(13) . . ? O25Y Cl21 O23X 86.8(2) . . ? O24Y Cl21 O23X 133.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11B Ag1 N11A C12A -74.6(6) . . . . ? N22B Ag1 N11A C12A 73.3(3) . . . . ? N22A Ag1 N11A C12A -172.7(3) . . . . ? N11B Ag1 N11A C16A 108.2(5) . . . . ? N22B Ag1 N11A C16A -104.0(2) . . . . ? N22A Ag1 N11A C16A 10.1(2) . . . . ? C16A N11A C12A C13A -0.7(5) . . . . ? Ag1 N11A C12A C13A -178.0(3) . . . . ? N11A C12A C13A C14A 1.4(6) . . . . ? C12A C13A C14A C15A -0.4(5) . . . . ? C13A C14A C15A C16A -1.3(5) . . . . ? C12A N11A C16A C15A -1.1(4) . . . . ? Ag1 N11A C16A C15A 176.4(2) . . . . ? C12A N11A C16A C23A 177.4(3) . . . . ? Ag1 N11A C16A C23A -5.1(3) . . . . ? C14A C15A C16A N11A 2.1(5) . . . . ? C14A C15A C16A C23A -176.4(3) . . . . ? C25A N21A N22A C23A 0.5(3) . . . . ? C26A N21A N22A C23A -179.1(2) . . . . ? C25A N21A N22A Ag1 157.7(2) . . . . ? C26A N21A N22A Ag1 -21.9(4) . . . . ? N11B Ag1 N22A C23A 177.24(19) . . . . ? N11A Ag1 N22A C23A -14.34(19) . . . . ? N22B Ag1 N22A C23A 97.9(2) . . . . ? N11B Ag1 N22A N21A 21.4(3) . . . . ? N11A Ag1 N22A N21A -170.2(3) . . . . ? N22B Ag1 N22A N21A -58.0(3) . . . . ? N21A N22A C23A C24A -0.8(3) . . . . ? Ag1 N22A C23A C24A -164.2(2) . . . . ? N21A N22A C23A C16A -178.9(2) . . . . ? Ag1 N22A C23A C16A 17.6(3) . . . . ? N11A C16A C23A N22A -8.9(4) . . . . ? C15A C16A C23A N22A 169.6(3) . . . . ? N11A C16A C23A C24A 173.3(3) . . . . ? C15A C16A C23A C24A -8.1(5) . . . . ? N22A C23A C24A C25A 0.8(4) . . . . ? C16A C23A C24A C25A 178.6(3) . . . . ? N22A N21A C25A C24A 0.0(3) . . . . ? C26A N21A C25A C24A 179.5(3) . . . . ? C23A C24A C25A N21A -0.4(3) . . . . ? N22A N21A C26A C51A 75.8(3) . . . . ? C25A N21A C26A C51A -103.7(3) . . . . ? N31B Ag2 N31A C32A -61.0(5) . . . . ? N42B Ag2 N31A C32A 56.3(3) . . . . ? N42A Ag2 N31A C32A -174.9(3) . . . . ? N31B Ag2 N31A C36A 124.3(4) . . . . ? N42B Ag2 N31A C36A -118.5(2) . . . . ? N42A Ag2 N31A C36A 10.3(2) . . . . ? C36A N31A C32A C33A 0.7(5) . . . . ? Ag2 N31A C32A C33A -174.0(3) . . . . ? N31A C32A C33A C34A -2.1(5) . . . . ? C32A C33A C34A C35A 1.2(6) . . . . ? C33A C34A C35A C36A 0.8(5) . . . . ? C32A N31A C36A C35A 1.4(5) . . . . ? Ag2 N31A C36A C35A 176.6(2) . . . . ? C32A N31A C36A C43A -177.8(3) . . . . ? Ag2 N31A C36A C43A -2.6(4) . . . . ? C34A C35A C36A N31A -2.2(5) . . . . ? C34A C35A C36A C43A 177.0(3) . . . . ? C45A N41A N42A C43A 1.5(4) . . . . ? C46A N41A N42A C43A 176.2(3) . . . . ? C45A N41A N42A Ag2 147.3(3) . . . . ? C46A N41A N42A Ag2 -38.1(5) . . . . ? N31B Ag2 N42A C43A 177.5(2) . . . . ? N31A Ag2 N42A C43A -17.2(2) . . . . ? N42B Ag2 N42A C43A 90.3(2) . . . . ? N31B Ag2 N42A N41A 32.8(3) . . . . ? N31A Ag2 N42A N41A -161.9(3) . . . . ? N42B Ag2 N42A N41A -54.5(4) . . . . ? N41A N42A C43A C44A -1.2(4) . . . . ? Ag2 N42A C43A C44A -157.4(2) . . . . ? N41A N42A C43A C36A 179.3(3) . . . . ? Ag2 N42A C43A C36A 23.0(3) . . . . ? N31A C36A C43A N42A -15.3(4) . . . . ? C35A C36A C43A N42A 165.5(3) . . . . ? N31A C36A C43A C44A 165.3(3) . . . . ? C35A C36A C43A C44A -13.9(5) . . . . ? N42A C43A C44A C45A 0.4(4) . . . . ? C36A C43A C44A C45A 179.9(3) . . . . ? N42A N41A C45A C44A -1.3(4) . . . . ? C46A N41A C45A C44A -175.3(3) . . . . ? C43A C44A C45A N41A 0.5(4) . . . . ? C45A N41A C46A C54A -113.5(4) . . . . ? N42A N41A C46A C54A 72.9(4) . . . . ? N21A C26A C51A C52A 3.2(4) . . . . ? N21A C26A C51A C56A -177.1(3) . . . . ? C56A C51A C52A C53A -0.7(4) . . . . ? C26A C51A C52A C53A 179.0(3) . . . . ? C51A C52A C53A C54A 0.4(5) . . . . ? C52A C53A C54A C55A 0.7(5) . . . . ? C52A C53A C54A C46A -177.6(3) . . . . ? N41A C46A C54A C53A 2.9(5) . . . . ? N41A C46A C54A C55A -175.5(3) . . . . ? C53A C54A C55A C61A 179.6(3) . . . . ? C46A C54A C55A C61A -2.0(5) . . . . ? C53A C54A C55A C56A -1.3(4) . . . . ? C46A C54A C55A C56A 177.1(3) . . . . ? C52A C51A C56A C64A 179.3(3) . . . . ? C26A C51A C56A C64A -0.5(4) . . . . ? C52A C51A C56A C55A 0.1(4) . . . . ? C26A C51A C56A C55A -179.7(3) . . . . ? C61A C55A C56A C64A 0.8(4) . . . . ? C54A C55A C56A C64A -178.3(3) . . . . ? C61A C55A C56A C51A -180.0(3) . . . . ? C54A C55A C56A C51A 1.0(4) . . . . ? C54A C55A C61A C62A 178.6(3) . . . . ? C56A C55A C61A C62A -0.5(5) . . . . ? C55A C61A C62A C63A -0.6(6) . . . . ? C61A C62A C63A C64A 1.3(6) . . . . ? C62A C63A C64A C56A -1.0(6) . . . . ? C51A C56A C64A C63A -179.3(3) . . . . ? C55A C56A C64A C63A 0.0(5) . . . . ? N11A Ag1 N11B C12B -32.7(6) . . . . ? N22B Ag1 N11B C12B 176.9(3) . . . . ? N22A Ag1 N11B C12B 61.4(3) . . . . ? N11A Ag1 N11B C16B 155.0(4) . . . . ? N22B Ag1 N11B C16B 4.6(2) . . . . ? N22A Ag1 N11B C16B -110.9(2) . . . . ? C16B N11B C12B C13B -0.5(5) . . . . ? Ag1 N11B C12B C13B -172.8(3) . . . . ? N11B C12B C13B C14B 0.2(6) . . . . ? C12B C13B C14B C15B 0.4(6) . . . . ? C13B C14B C15B C16B -0.8(6) . . . . ? C12B N11B C16B C15B 0.1(4) . . . . ? Ag1 N11B C16B C15B 172.9(2) . . . . ? C12B N11B C16B C23B 179.3(3) . . . . ? Ag1 N11B C16B C23B -7.9(3) . . . . ? C14B C15B C16B N11B 0.5(5) . . . . ? C14B C15B C16B C23B -178.7(3) . . . . ? C25B N21B N22B C23B 0.3(3) . . . . ? C26B N21B N22B C23B -176.4(3) . . . . ? C25B N21B N22B Ag1 -171.7(3) . . . . ? C26B N21B N22B Ag1 11.6(4) . . . . ? N11B Ag1 N22B C23B -0.66(19) . . . . ? N11A Ag1 N22B C23B -174.53(19) . . . . ? N22A Ag1 N22B C23B 102.9(2) . . . . ? N11B Ag1 N22B N21B 170.8(3) . . . . ? N11A Ag1 N22B N21B -3.0(3) . . . . ? N22A Ag1 N22B N21B -85.6(3) . . . . ? N21B N22B C23B C24B -0.1(3) . . . . ? Ag1 N22B C23B C24B 174.3(2) . . . . ? N21B N22B C23B C16B -177.4(3) . . . . ? Ag1 N22B C23B C16B -3.1(3) . . . . ? N11B C16B C23B N22B 7.4(4) . . . . ? C15B C16B C23B N22B -173.4(3) . . . . ? N11B C16B C23B C24B -169.4(3) . . . . ? C15B C16B C23B C24B 9.9(5) . . . . ? N22B C23B C24B C25B -0.2(4) . . . . ? C16B C23B C24B C25B 176.8(3) . . . . ? N22B N21B C25B C24B -0.4(4) . . . . ? C26B N21B C25B C24B 175.9(3) . . . . ? C23B C24B C25B N21B 0.4(4) . . . . ? C25B N21B C26B C51B -93.8(4) . . . . ? N22B N21B C26B C51B 82.2(3) . . . . ? N31A Ag2 N31B C32B -71.6(5) . . . . ? N42B Ag2 N31B C32B 166.1(3) . . . . ? N42A Ag2 N31B C32B 37.1(3) . . . . ? N31A Ag2 N31B C36B 119.1(4) . . . . ? N42B Ag2 N31B C36B -3.2(2) . . . . ? N42A Ag2 N31B C36B -132.2(2) . . . . ? C36B N31B C32B C33B -0.7(5) . . . . ? Ag2 N31B C32B C33B -170.0(3) . . . . ? N31B C32B C33B C34B -0.6(6) . . . . ? C32B C33B C34B C35B 0.7(5) . . . . ? C33B C34B C35B C36B 0.5(5) . . . . ? C32B N31B C36B C35B 1.9(4) . . . . ? Ag2 N31B C36B C35B 172.1(2) . . . . ? C32B N31B C36B C43B -175.5(3) . . . . ? Ag2 N31B C36B C43B -5.3(3) . . . . ? C34B C35B C36B N31B -1.8(5) . . . . ? C34B C35B C36B C43B 175.5(3) . . . . ? C45B N41B N42B C43B -0.7(3) . . . . ? C46B N41B N42B C43B -175.7(3) . . . . ? C45B N41B N42B Ag2 -155.9(2) . . . . ? C46B N41B N42B Ag2 29.2(4) . . . . ? N31B Ag2 N42B C43B 11.6(2) . . . . ? N31A Ag2 N42B C43B -154.6(2) . . . . ? N42A Ag2 N42B C43B 117.9(2) . . . . ? N31B Ag2 N42B N41B 165.9(3) . . . . ? N31A Ag2 N42B N41B -0.3(3) . . . . ? N42A Ag2 N42B N41B -87.8(3) . . . . ? N41B N42B C43B C44B 0.6(3) . . . . ? Ag2 N42B C43B C44B 164.0(2) . . . . ? N41B N42B C43B C36B 177.4(3) . . . . ? Ag2 N42B C43B C36B -19.1(3) . . . . ? N31B C36B C43B N42B 17.5(4) . . . . ? C35B C36B C43B N42B -159.9(3) . . . . ? N31B C36B C43B C44B -166.3(3) . . . . ? C35B C36B C43B C44B 16.3(5) . . . . ? N42B C43B C44B C45B -0.2(4) . . . . ? C36B C43B C44B C45B -176.7(3) . . . . ? N42B N41B C45B C44B 0.6(4) . . . . ? C46B N41B C45B C44B 174.9(3) . . . . ? C43B C44B C45B N41B -0.2(4) . . . . ? C45B N41B C46B C54B -109.1(4) . . . . ? N42B N41B C46B C54B 64.8(4) . . . . ? N21B C26B C51B C52B -86.9(3) . . . . ? N21B C26B C51B C56B 92.3(3) . . . . ? C56B C51B C52B C53B -3.2(4) . . . . ? C26B C51B C52B C53B 176.0(3) . . . . ? C51B C52B C53B C54B 1.0(5) . . . . ? C52B C53B C54B C55B 3.2(5) . . . . ? C52B C53B C54B C46B -176.4(3) . . . . ? N41B C46B C54B C53B 42.2(4) . . . . ? N41B C46B C54B C55B -137.3(3) . . . . ? C53B C54B C55B C61B 174.3(3) . . . . ? C46B C54B C55B C61B -6.1(5) . . . . ? C53B C54B C55B C56B -5.1(4) . . . . ? C46B C54B C55B C56B 174.5(3) . . . . ? C52B C51B C56B C64B -177.1(3) . . . . ? C26B C51B C56B C64B 3.7(4) . . . . ? C52B C51B C56B C55B 1.3(4) . . . . ? C26B C51B C56B C55B -177.9(3) . . . . ? C61B C55B C56B C64B 1.8(4) . . . . ? C54B C55B C56B C64B -178.8(3) . . . . ? C61B C55B C56B C51B -176.6(3) . . . . ? C54B C55B C56B C51B 2.8(4) . . . . ? C54B C55B C61B C62B -179.5(3) . . . . ? C56B C55B C61B C62B -0.1(5) . . . . ? C55B C61B C62B C63B -1.6(5) . . . . ? C61B C62B C63B C64B 1.6(6) . . . . ? C62B C63B C64B C56B 0.2(5) . . . . ? C51B C56B C64B C63B 176.5(3) . . . . ? C55B C56B C64B C63B -1.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.14 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.972 _refine_diff_density_min -1.084 _refine_diff_density_rms 0.072 data_imw1686newcell _database_code_depnum_ccdc_archive 'CCDC 895601' #TrackingRef 'Ag_Ward_Stephenson_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C25 H22 Ag N6 O), C7H8, 2(B F4)' _chemical_formula_sum 'C57 H52 Ag2 B2 F8 N12 O2' _chemical_formula_weight 1326.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4096(4) _cell_length_b 11.3764(5) _cell_length_c 23.0044(11) _cell_angle_alpha 90.00 _cell_angle_beta 92.754(3) _cell_angle_gamma 90.00 _cell_volume 2721.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3830 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 22.12 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8958 _exptl_absorpt_correction_T_max 0.9534 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18519 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3888 _reflns_number_gt 2412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. It is a 1-dimensional coordination polymer composed of a continuous Ag - ligand chain, with one tetrafluoroborate anion and half a toluene molecule per Ag. All hydrogens were added in calculated positions. There is a discrepancy between calculated and reported formulae. This is because the toluene molecule lies over a two-fold axis such that only 5 carbons are present in the asymmetric unit. Of these three were made half occupancy and 4 were left full occupancy so that the total is seven carbons. However because some carbons had effectively two different hybridisations it was not possible to add the hydrogens precisely and they were left out of the refinement. Therefore there is a discrepancy of 8 hydrogens per every Ag2 unit. The tetrafluoroborate anion was disordered along the B1 - F1 axis such that three of the F atoms were disordered over two sites: [F2 > F4 and F5 > F7 (58 : 42)]. All 6 and 5 membered rings were fixed using geometric restraints as was the tetrafluoroborate anion. Global displacement restraints have been used to achieve a consistent model. The crystals were relatively weakly diffracting and the data was cut at an appropriate point. 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^)+(0.0834P)^2^+14.5209P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3888 _refine_ls_number_parameters 363 _refine_ls_number_restraints 430 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1891 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.079 _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 0.85931(6) 0.88315(7) 0.12959(4) 0.0502(3) Uani 1 1 d . . . N111 N 0.9006(5) 1.0361(4) 0.0616(2) 0.0388(17) Uani 1 1 d GU . . C112 C 1.0005(4) 1.1103(5) 0.08009(19) 0.0345(18) Uani 1 1 d GU . . C113 C 1.0278(5) 1.2097(5) 0.0478(3) 0.045(2) Uani 1 1 d GU . . H113 H 1.0947 1.2594 0.0602 0.054 Uiso 1 1 calc R . . C114 C 0.9553(6) 1.2349(5) -0.0030(2) 0.056(3) Uani 1 1 d GU . . H114 H 0.9736 1.3014 -0.0246 0.068 Uiso 1 1 calc R . . C115 C 0.8554(5) 1.1607(6) -0.0215(2) 0.054(2) Uani 1 1 d GU . . H115 H 0.8069 1.1775 -0.0554 0.065 Uiso 1 1 calc R . . C116 C 0.8281(4) 1.0613(5) 0.0108(2) 0.050(2) Uani 1 1 d GU . . H116 H 0.7613 1.0116 -0.0015 0.060 Uiso 1 1 calc R . . N121 N 1.1420(4) 0.9500(4) 0.2010(2) 0.0358(16) Uani 1 1 d GU . . N122 N 1.0510(4) 0.9653(4) 0.1536(2) 0.0324(16) Uani 1 1 d GU . . C123 C 1.0728(5) 1.0772(4) 0.1285(2) 0.0309(18) Uani 1 1 d GU . . C124 C 1.1772(5) 1.1309(4) 0.1603(3) 0.041(2) Uani 1 1 d GU . . H124 H 1.2115 1.2047 0.1531 0.049 Uiso 1 1 calc R . . C125 C 1.2200(4) 1.0523(5) 0.2051(2) 0.043(2) Uani 1 1 d GU . . H125 H 1.2873 1.0656 0.2324 0.052 Uiso 1 1 calc R . . C126 C 1.1570(8) 0.8429(8) 0.2295(4) 0.039(2) Uani 1 1 d U . . H12A H 1.2231 0.8507 0.2605 0.047 Uiso 1 1 calc R . . H12B H 1.1860 0.7846 0.2023 0.047 Uiso 1 1 calc R . . C131 C 1.0344(5) 0.8000(5) 0.2551(3) 0.045(2) Uani 1 1 d GU . . C132 C 0.9706(5) 0.7015(5) 0.2326(2) 0.051(2) Uani 1 1 d GU . . H132 H 1.0013 0.6629 0.2005 0.062 Uiso 1 1 calc R . . C133 C 0.8608(5) 0.6607(5) 0.2582(3) 0.060(3) Uani 1 1 d GU . . C134 C 0.8149(5) 0.7184(6) 0.3063(3) 0.072(3) Uani 1 1 d GU . . H134 H 0.7415 0.6911 0.3234 0.087 Uiso 1 1 calc R . . C135 C 0.8788(6) 0.8169(6) 0.3287(3) 0.077(3) Uani 1 1 d GU . . C136 C 0.9885(6) 0.8577(5) 0.3031(3) 0.065(3) Uani 1 1 d GU . . H136 H 1.0313 0.9236 0.3182 0.078 Uiso 1 1 calc R . . O137 O 0.8413(11) 0.8820(9) 0.3748(5) 0.130(4) Uani 1 1 d . . . C138 C 0.7359(15) 0.8377(16) 0.4068(8) 0.147(8) Uani 1 1 d . . . H13A H 0.7544 0.7587 0.4193 0.221 Uiso 1 1 calc R . . H13B H 0.6587 0.8383 0.3823 0.221 Uiso 1 1 calc R . . H13C H 0.7244 0.8865 0.4402 0.221 Uiso 1 1 calc R . . N211 N 0.7204(5) 0.7397(6) 0.1045(3) 0.056(2) Uani 1 1 d GDU . . C212 C 0.6092(5) 0.7326(5) 0.1354(2) 0.049(2) Uani 1 1 d GDU . . C213 C 0.5114(5) 0.6557(7) 0.1174(4) 0.089(4) Uani 1 1 d GDU . . H213 H 0.4370 0.6509 0.1381 0.107 Uiso 1 1 calc R . . C214 C 0.5249(7) 0.5859(8) 0.0685(4) 0.133(5) Uani 1 1 d GDU . . H214 H 0.4595 0.5345 0.0564 0.160 Uiso 1 1 calc R . . C215 C 0.6361(8) 0.5930(8) 0.0376(3) 0.136(5) Uani 1 1 d GDU . . H215 H 0.6451 0.5464 0.0048 0.164 Uiso 1 1 calc R . . C216 C 0.7339(6) 0.6699(8) 0.0556(3) 0.098(4) Uani 1 1 d GDU . . H216 H 0.8083 0.6747 0.0349 0.118 Uiso 1 1 calc R . . N221 N 0.6489(5) 0.9503(5) 0.2458(3) 0.059(2) Uani 1 1 d GDU . . N222 N 0.6834(4) 0.8944(5) 0.1937(2) 0.0413(17) Uani 1 1 d GDU . . C223 C 0.5982(5) 0.7985(5) 0.1830(2) 0.042(2) Uani 1 1 d GDU . . C224 C 0.5110(5) 0.7952(5) 0.2285(3) 0.053(2) Uani 1 1 d GDU . . H224 H 0.4449 0.7410 0.2323 0.064 Uiso 1 1 calc R . . C225 C 0.5423(6) 0.8890(6) 0.2674(2) 0.065(3) Uani 1 1 d GDU . . H225 H 0.5004 0.9070 0.3011 0.078 Uiso 1 1 calc R . . C226 C 0.7055(9) 1.0513(10) 0.2663(6) 0.071(3) Uani 1 1 d DU . . H22A H 0.7949 1.0521 0.2562 0.085 Uiso 1 1 calc R . . H22B H 0.7035 1.0526 0.3085 0.085 Uiso 1 1 calc R . . B1 B 0.1660(9) 0.5188(8) 0.1137(4) 0.047(2) Uani 1 1 d DU . . F1 F 0.0345(5) 0.5284(7) 0.1108(2) 0.082(2) Uani 1 1 d DU A . F2 F 0.2049(14) 0.4948(19) 0.0607(5) 0.082(5) Uani 0.58(3) 1 d PDU A 1 F3 F 0.2142(13) 0.6222(12) 0.1326(11) 0.095(6) Uani 0.58(3) 1 d PDU A 1 F4 F 0.1964(13) 0.4326(16) 0.1510(7) 0.082(5) Uani 0.58(3) 1 d PDU A 1 F5 F 0.2195(15) 0.560(3) 0.0644(7) 0.070(6) Uani 0.42(3) 1 d PDU A 2 F6 F 0.2221(14) 0.580(2) 0.1616(8) 0.071(6) Uani 0.42(3) 1 d PDU A 2 F7 F 0.2039(18) 0.4024(12) 0.1209(14) 0.111(8) Uani 0.42(3) 1 d PDU A 2 C1 C 0.492(2) 0.860(3) 1.0128(14) 0.088(7) Uani 0.50 1 d PU . . C2 C 0.516(3) 0.819(3) 0.9571(15) 0.101(6) Uani 0.50 1 d PU . . C3 C 0.542(3) 0.879(4) 0.9158(16) 0.105(6) Uani 0.50 1 d PU . . C4 C 0.5359(15) 0.984(2) 0.9229(8) 0.120(5) Uani 1 1 d U . . C5 C 0.5101(13) 1.0402(19) 0.9742(7) 0.111(5) Uani 1 1 d U . . 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 0.0281(4) 0.0465(5) 0.0762(6) 0.0054(4) 0.0060(3) -0.0118(3) N111 0.030(4) 0.047(5) 0.040(4) -0.001(4) 0.005(3) 0.004(3) C112 0.035(4) 0.034(4) 0.035(4) 0.001(4) 0.009(3) 0.005(4) C113 0.038(5) 0.043(5) 0.055(5) 0.010(4) 0.013(4) 0.004(4) C114 0.049(5) 0.065(6) 0.056(6) 0.022(5) 0.021(4) 0.011(5) C115 0.049(5) 0.072(6) 0.041(5) 0.011(5) 0.010(4) 0.020(5) C116 0.038(5) 0.064(6) 0.049(5) -0.003(5) 0.002(4) 0.008(4) N121 0.024(3) 0.039(4) 0.045(4) 0.004(3) 0.006(3) -0.002(3) N122 0.020(3) 0.038(4) 0.039(4) -0.001(3) 0.007(3) 0.000(3) C123 0.027(4) 0.027(4) 0.039(4) 0.003(4) 0.013(3) -0.002(3) C124 0.040(4) 0.030(5) 0.052(5) 0.001(4) 0.001(4) -0.006(4) C125 0.034(4) 0.041(5) 0.054(5) -0.005(4) 0.001(4) -0.005(4) C126 0.032(4) 0.037(5) 0.047(5) 0.017(4) 0.006(4) 0.002(4) C131 0.030(4) 0.048(5) 0.059(5) 0.022(4) 0.008(4) 0.004(4) C132 0.028(4) 0.058(6) 0.068(6) 0.028(5) 0.001(4) 0.004(4) C133 0.031(5) 0.060(6) 0.089(7) 0.044(5) 0.002(5) 0.000(4) C134 0.044(5) 0.069(7) 0.106(8) 0.054(6) 0.029(5) 0.008(5) C135 0.066(6) 0.066(7) 0.105(8) 0.037(6) 0.051(6) 0.016(5) C136 0.055(5) 0.057(6) 0.086(7) 0.026(5) 0.031(5) 0.011(5) O137 0.134(9) 0.101(8) 0.165(10) 0.019(7) 0.123(8) 0.017(6) C138 0.120(13) 0.161(16) 0.171(16) 0.074(14) 0.117(13) 0.034(12) N211 0.040(4) 0.064(5) 0.065(5) -0.016(4) 0.013(4) -0.014(4) C212 0.032(4) 0.054(5) 0.061(5) -0.016(4) 0.016(4) -0.015(4) C213 0.050(6) 0.100(8) 0.119(8) -0.054(7) 0.026(6) -0.037(6) C214 0.079(7) 0.162(10) 0.159(10) -0.106(8) 0.028(7) -0.052(7) C215 0.084(7) 0.178(11) 0.149(10) -0.105(9) 0.027(7) -0.046(8) C216 0.068(6) 0.125(9) 0.104(8) -0.064(7) 0.029(6) -0.027(6) N221 0.036(4) 0.063(5) 0.079(5) -0.019(4) 0.005(4) 0.014(4) N222 0.025(3) 0.045(4) 0.054(4) -0.007(4) -0.003(3) 0.005(3) C223 0.024(4) 0.046(5) 0.056(5) 0.002(4) 0.006(4) 0.002(4) C224 0.028(4) 0.062(6) 0.070(6) 0.006(5) 0.013(4) 0.008(4) C225 0.043(5) 0.079(7) 0.075(6) -0.006(6) 0.016(5) 0.013(5) C226 0.037(5) 0.072(7) 0.103(8) -0.048(6) -0.017(5) 0.009(5) B1 0.045(5) 0.053(6) 0.045(6) 0.006(5) 0.009(5) 0.001(5) F1 0.044(3) 0.140(6) 0.063(4) 0.015(4) 0.004(3) -0.009(4) F2 0.089(9) 0.097(13) 0.063(7) 0.009(8) 0.039(6) 0.004(9) F3 0.072(8) 0.065(8) 0.153(15) -0.026(9) 0.053(10) -0.027(7) F4 0.095(8) 0.080(10) 0.073(10) 0.034(8) 0.008(8) 0.029(7) F5 0.055(9) 0.093(15) 0.063(9) 0.043(9) 0.014(7) 0.014(10) F6 0.042(8) 0.111(14) 0.062(11) -0.034(10) 0.024(7) -0.020(9) F7 0.144(14) 0.038(9) 0.144(18) 0.007(11) -0.077(13) -0.003(9) C1 0.045(11) 0.116(18) 0.100(15) -0.009(15) -0.020(12) 0.002(12) C2 0.057(10) 0.140(16) 0.103(14) -0.021(13) -0.022(12) 0.002(11) C3 0.063(10) 0.149(15) 0.101(13) -0.023(13) -0.016(10) 0.011(12) C4 0.080(8) 0.169(14) 0.109(10) -0.031(10) -0.019(7) 0.018(10) C5 0.047(7) 0.180(16) 0.106(11) -0.038(11) -0.012(8) 0.022(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N211 2.237(5) . ? Ag1 N122 2.249(4) . ? Ag1 N111 2.392(4) . ? Ag1 N222 2.408(4) . ? N111 C112 1.3900 . ? N111 C116 1.3900 . ? C112 C123 1.366(5) . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C113 H113 0.9300 . ? C114 C115 1.3900 . ? C114 H114 0.9300 . ? C115 C116 1.3900 . ? C115 H115 0.9300 . ? C116 H116 0.9300 . ? N121 C126 1.389(9) . ? N121 N122 1.4200 . ? N121 C125 1.4200 . ? N122 C123 1.4200 . ? C123 C124 1.4200 . ? C124 C125 1.4200 . ? C124 H124 0.9300 . ? C125 H125 0.9300 . ? C126 C131 1.511(9) . ? C126 H12A 0.9700 . ? C126 H12B 0.9700 . ? C131 C132 1.3900 . ? C131 C136 1.3900 . ? C132 C133 1.3900 . ? C132 H132 0.9300 . ? C133 C134 1.3900 . ? C133 C226 1.519(13) 2_645 ? C134 C135 1.3900 . ? C134 H134 0.9300 . ? C135 O137 1.365(11) . ? C135 C136 1.3900 . ? C136 H136 0.9300 . ? O137 C138 1.441(14) . ? C138 H13A 0.9600 . ? C138 H13B 0.9600 . ? C138 H13C 0.9600 . ? N211 C212 1.3900 . ? N211 C216 1.3900 . ? C212 C223 1.335(6) . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C213 H213 0.9300 . ? C214 C215 1.3900 . ? C214 H214 0.9300 . ? C215 C216 1.3900 . ? C215 H215 0.9300 . ? C216 H216 0.9300 . ? N221 C226 1.366(11) . ? N221 C225 1.4200 . ? N221 N222 1.4200 . ? N222 C223 1.4200 . ? C223 C224 1.4200 . ? C224 C225 1.4200 . ? C224 H224 0.9300 . ? C225 H225 0.9300 . ? C226 C133 1.52(2) 2_655 ? C226 H22A 0.9700 . ? C226 H22B 0.9700 . ? B1 F4 1.332(13) . ? B1 F2 1.333(13) . ? B1 F3 1.342(13) . ? B1 F5 1.371(14) . ? B1 F1 1.372(10) . ? B1 F7 1.390(15) . ? B1 F6 1.404(14) . ? C1 C5 1.17(3) 3_677 ? C1 C2 1.40(4) . ? C2 C3 1.21(4) . ? C3 C4 1.20(4) . ? C4 C5 1.38(2) . ? C5 C1 1.17(3) 3_677 ? C5 C5 1.52(4) 3_677 ? 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 N211 Ag1 N122 157.2(2) . . ? N211 Ag1 N111 119.8(2) . . ? N122 Ag1 N111 70.90(17) . . ? N211 Ag1 N222 72.27(19) . . ? N122 Ag1 N222 121.29(18) . . ? N111 Ag1 N222 121.83(19) . . ? C112 N111 C116 120.0 . . ? C112 N111 Ag1 113.4(3) . . ? C116 N111 Ag1 126.3(3) . . ? C123 C112 N111 117.1(4) . . ? C123 C112 C113 122.8(4) . . ? N111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C115 C114 C113 120.0 . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C115 C116 N111 120.0 . . ? C115 C116 H116 120.0 . . ? N111 C116 H116 120.0 . . ? C126 N121 N122 121.7(5) . . ? C126 N121 C125 129.5(5) . . ? N122 N121 C125 108.0 . . ? N121 N122 C123 108.0 . . ? N121 N122 Ag1 133.5(3) . . ? C123 N122 Ag1 115.4(3) . . ? C112 C123 N122 119.1(4) . . ? C112 C123 C124 132.8(4) . . ? N122 C123 C124 108.0 . . ? C123 C124 C125 108.0 . . ? C123 C124 H124 126.0 . . ? C125 C124 H124 126.0 . . ? N121 C125 C124 108.0 . . ? N121 C125 H125 126.0 . . ? C124 C125 H125 126.0 . . ? N121 C126 C131 112.9(6) . . ? N121 C126 H12A 109.0 . . ? C131 C126 H12A 109.0 . . ? N121 C126 H12B 109.0 . . ? C131 C126 H12B 109.0 . . ? H12A C126 H12B 107.8 . . ? C132 C131 C136 120.0 . . ? C132 C131 C126 120.9(5) . . ? C136 C131 C126 119.1(5) . . ? C133 C132 C131 120.0 . . ? C133 C132 H132 120.0 . . ? C131 C132 H132 120.0 . . ? C134 C133 C132 120.0 . . ? C134 C133 C226 121.0(6) . 2_645 ? C132 C133 C226 119.0(6) . 2_645 ? C133 C134 C135 120.0 . . ? C133 C134 H134 120.0 . . ? C135 C134 H134 120.0 . . ? O137 C135 C136 114.8(6) . . ? O137 C135 C134 125.2(6) . . ? C136 C135 C134 120.0 . . ? C135 C136 C131 120.0 . . ? C135 C136 H136 120.0 . . ? C131 C136 H136 120.0 . . ? C135 O137 C138 117.4(12) . . ? O137 C138 H13A 109.5 . . ? O137 C138 H13B 109.5 . . ? H13A C138 H13B 109.5 . . ? O137 C138 H13C 109.5 . . ? H13A C138 H13C 109.5 . . ? H13B C138 H13C 109.5 . . ? C212 N211 C216 120.0 . . ? C212 N211 Ag1 117.0(3) . . ? C216 N211 Ag1 122.4(3) . . ? C223 C212 N211 119.5(4) . . ? C223 C212 C213 120.5(4) . . ? N211 C212 C213 120.0 . . ? C212 C213 C214 120.0 . . ? C212 C213 H213 120.0 . . ? C214 C213 H213 120.0 . . ? C215 C214 C213 120.0 . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C216 C215 C214 120.0 . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C215 C216 N211 120.0 . . ? C215 C216 H216 120.0 . . ? N211 C216 H216 120.0 . . ? C226 N221 C225 128.6(7) . . ? C226 N221 N222 123.1(7) . . ? C225 N221 N222 108.0 . . ? C223 N222 N221 108.0 . . ? C223 N222 Ag1 109.9(3) . . ? N221 N222 Ag1 140.5(3) . . ? C212 C223 N222 119.7(5) . . ? C212 C223 C224 132.2(5) . . ? N222 C223 C224 108.0 . . ? C225 C224 C223 108.0 . . ? C225 C224 H224 126.0 . . ? C223 C224 H224 126.0 . . ? C224 C225 N221 108.0 . . ? C224 C225 H225 126.0 . . ? N221 C225 H225 126.0 . . ? N221 C226 C133 112.4(8) . 2_655 ? N221 C226 H22A 109.1 . . ? C133 C226 H22A 109.1 2_655 . ? N221 C226 H22B 109.1 . . ? C133 C226 H22B 109.1 2_655 . ? H22A C226 H22B 107.9 . . ? F4 B1 F2 111.4(10) . . ? F4 B1 F3 111.3(10) . . ? F2 B1 F3 110.5(9) . . ? F4 B1 F5 133.8(12) . . ? F2 B1 F5 32.6(9) . . ? F3 B1 F5 79.0(11) . . ? F4 B1 F1 107.2(9) . . ? F2 B1 F1 108.5(9) . . ? F3 B1 F1 107.6(9) . . ? F5 B1 F1 112.1(9) . . ? F4 B1 F7 33.2(10) . . ? F2 B1 F7 79.4(12) . . ? F3 B1 F7 134.2(12) . . ? F5 B1 F7 107.4(11) . . ? F1 B1 F7 111.0(10) . . ? F4 B1 F6 77.5(11) . . ? F2 B1 F6 133.3(11) . . ? F3 B1 F6 34.7(9) . . ? F5 B1 F6 108.0(10) . . ? F1 B1 F6 112.1(9) . . ? F7 B1 F6 105.9(10) . . ? C5 C1 C2 124(3) 3_677 . ? C3 C2 C1 126(4) . . ? C4 C3 C2 116(4) . . ? C3 C4 C5 126(3) . . ? C1 C5 C4 132(3) 3_677 . ? C1 C5 C5 112(3) 3_677 3_677 ? C4 C5 C5 115(2) . 3_677 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N211 Ag1 N111 C112 -172.2(3) . . . . ? N122 Ag1 N111 C112 -14.5(3) . . . . ? N222 Ag1 N111 C112 101.1(3) . . . . ? N211 Ag1 N111 C116 14.3(4) . . . . ? N122 Ag1 N111 C116 172.0(3) . . . . ? N222 Ag1 N111 C116 -72.4(4) . . . . ? C116 N111 C112 C123 -176.4(5) . . . . ? Ag1 N111 C112 C123 9.6(5) . . . . ? C116 N111 C112 C113 0.0 . . . . ? Ag1 N111 C112 C113 -174.0(3) . . . . ? C123 C112 C113 C114 176.2(6) . . . . ? N111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 N111 0.0 . . . . ? C112 N111 C116 C115 0.0 . . . . ? Ag1 N111 C116 C115 173.2(4) . . . . ? C126 N121 N122 C123 -171.1(6) . . . . ? C125 N121 N122 C123 0.0 . . . . ? C126 N121 N122 Ag1 30.2(7) . . . . ? C125 N121 N122 Ag1 -158.7(5) . . . . ? N211 Ag1 N122 N121 -63.0(7) . . . . ? N111 Ag1 N122 N121 174.9(4) . . . . ? N222 Ag1 N122 N121 58.6(4) . . . . ? N211 Ag1 N122 C123 139.5(5) . . . . ? N111 Ag1 N122 C123 17.4(3) . . . . ? N222 Ag1 N122 C123 -98.9(3) . . . . ? N111 C112 C123 N122 6.1(6) . . . . ? C113 C112 C123 N122 -170.2(3) . . . . ? N111 C112 C123 C124 -177.8(4) . . . . ? C113 C112 C123 C124 6.0(7) . . . . ? N121 N122 C123 C112 177.0(6) . . . . ? Ag1 N122 C123 C112 -19.9(5) . . . . ? N121 N122 C123 C124 0.0 . . . . ? Ag1 N122 C123 C124 163.1(4) . . . . ? C112 C123 C124 C125 -176.4(7) . . . . ? N122 C123 C124 C125 0.0 . . . . ? C126 N121 C125 C124 170.1(7) . . . . ? N122 N121 C125 C124 0.0 . . . . ? C123 C124 C125 N121 0.0 . . . . ? N122 N121 C126 C131 -58.4(9) . . . . ? C125 N121 C126 C131 132.6(6) . . . . ? N121 C126 C131 C132 111.6(7) . . . . ? N121 C126 C131 C136 -70.9(8) . . . . ? C136 C131 C132 C133 0.0 . . . . ? C126 C131 C132 C133 177.4(6) . . . . ? C131 C132 C133 C134 0.0 . . . . ? C131 C132 C133 C226 -178.7(7) . . . 2_645 ? C132 C133 C134 C135 0.0 . . . . ? C226 C133 C134 C135 178.6(7) 2_645 . . . ? C133 C134 C135 O137 178.5(9) . . . . ? C133 C134 C135 C136 0.0 . . . . ? O137 C135 C136 C131 -178.7(8) . . . . ? C134 C135 C136 C131 0.0 . . . . ? C132 C131 C136 C135 0.0 . . . . ? C126 C131 C136 C135 -177.5(6) . . . . ? C136 C135 O137 C138 -174.0(10) . . . . ? C134 C135 O137 C138 7.4(16) . . . . ? N122 Ag1 N211 C212 131.9(5) . . . . ? N111 Ag1 N211 C212 -115.4(4) . . . . ? N222 Ag1 N211 C212 1.7(4) . . . . ? N122 Ag1 N211 C216 -56.6(7) . . . . ? N111 Ag1 N211 C216 56.1(4) . . . . ? N222 Ag1 N211 C216 173.2(4) . . . . ? C216 N211 C212 C223 178.8(6) . . . . ? Ag1 N211 C212 C223 -9.4(7) . . . . ? C216 N211 C212 C213 0.0 . . . . ? Ag1 N211 C212 C213 171.7(5) . . . . ? C223 C212 C213 C214 -178.8(7) . . . . ? N211 C212 C213 C214 0.0 . . . . ? C212 C213 C214 C215 0.0 . . . . ? C213 C214 C215 C216 0.0 . . . . ? C214 C215 C216 N211 0.0 . . . . ? C212 N211 C216 C215 0.0 . . . . ? Ag1 N211 C216 C215 -171.3(5) . . . . ? C226 N221 N222 C223 -174.9(8) . . . . ? C225 N221 N222 C223 0.0 . . . . ? C226 N221 N222 Ag1 21.9(10) . . . . ? C225 N221 N222 Ag1 -163.2(6) . . . . ? N211 Ag1 N222 C223 5.2(3) . . . . ? N122 Ag1 N222 C223 -154.5(3) . . . . ? N111 Ag1 N222 C223 119.8(3) . . . . ? N211 Ag1 N222 N221 168.2(6) . . . . ? N122 Ag1 N222 N221 8.6(6) . . . . ? N111 Ag1 N222 N221 -77.2(5) . . . . ? N211 C212 C223 N222 15.2(8) . . . . ? C213 C212 C223 N222 -165.9(4) . . . . ? N211 C212 C223 C224 -166.4(5) . . . . ? C213 C212 C223 C224 12.5(8) . . . . ? N221 N222 C223 C212 178.8(7) . . . . ? Ag1 N222 C223 C212 -12.5(6) . . . . ? N221 N222 C223 C224 0.0 . . . . ? Ag1 N222 C223 C224 168.7(4) . . . . ? C212 C223 C224 C225 -178.5(8) . . . . ? N222 C223 C224 C225 0.0 . . . . ? C223 C224 C225 N221 0.0 . . . . ? C226 N221 C225 C224 174.5(9) . . . . ? N222 N221 C225 C224 0.0 . . . . ? C225 N221 C226 C133 -85.7(14) . . . 2_655 ? N222 N221 C226 C133 88.1(12) . . . 2_655 ? C5 C1 C2 C3 3(5) 3_677 . . . ? C1 C2 C3 C4 -6(5) . . . . ? C2 C3 C4 C5 4(4) . . . . ? C3 C4 C5 C1 176(3) . . . 3_677 ? C3 C4 C5 C5 1(3) . . . 3_677 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.939 _refine_diff_density_min -0.885 _refine_diff_density_rms 0.141 data_imw1713c2c _database_code_depnum_ccdc_archive 'CCDC 895602' #TrackingRef 'Ag_Ward_Stephenson_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C120 H96 Ag4 N32, 2(C7 H8), 4(B F4)' _chemical_formula_sum 'C134 H112 Ag4 B4 F16 N32' _chemical_formula_weight 2949.28 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.111(6) _cell_length_b 11.236(2) _cell_length_c 40.686(8) _cell_angle_alpha 90.00 _cell_angle_beta 111.635(2) _cell_angle_gamma 90.00 _cell_volume 14495(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5805 _cell_measurement_theta_min 4.50 _cell_measurement_theta_max 21.25 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5968 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8825 _exptl_absorpt_correction_T_max 0.9140 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67114 _diffrn_reflns_av_R_equivalents 0.1137 _diffrn_reflns_av_sigmaI/netI 0.2184 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 4.40 _diffrn_reflns_theta_max 27.68 _reflns_number_total 16197 _reflns_number_gt 7674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. It is a [Ag4(C30H24N8)4][BF4]4 complex with two toluene solvent molecules per Ag4 complex. The space group was confirmed by Platon. All hydrogens were added in calculated positions. One of the azo-groups (the only one completely within the asymmetric unit) was disordered over two sites: N171,N172 and N173,N174 (42:58). One of the two [BF4] anions was also disordered such that the two components shared three fluorine atoms but there was two boron and two fluorine atoms disordered: B11,F12 and B11X,F12X (60:40). One toluene molecule lies over a two-fold axis such that only 4 carbons are present in the asymmetric unit. Of these one was made half occupancy and 3 were left full occupancy. However because the CH3 carbon was disordered over two sites it was not possible to add the hydrogens precisely and they were left out of the refinement.Therefore there is a discrepency of 8 hydrogens per every Ag4 unit. This has caused a difference between expected and reported formulae which is seen in the cif check. The other toluene molecule was also made half occupancy. The structure contained solvent accessible voids and therefore the Platon Squeeze program was employed: loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.010 0.925 0.161 14 1 ' ' 2 0.010 0.925 0.339 14 1 ' ' 3 -0.010 0.075 0.661 14 1 ' ' 4 0.010 0.075 0.839 14 1 ' ' 5 0.250 0.750 0.000 363 41 ' ' 6 0.250 0.250 0.500 363 41 ' ' 7 0.490 0.425 0.161 14 1 ' ' 8 0.490 0.575 0.661 14 1 ' ' 9 0.510 0.425 0.339 14 1 ' ' 10 0.510 0.575 0.839 14 1 ' ' 11 0.750 0.250 0.000 363 41 ' ' 12 0.750 0.750 0.500 363 41 ' ' _platon_squeeze_details All 6 and 5 membered rings were fixed using geometric restraints as were the anions and one toluene solvent molecule. Global displacement restraints have been used to achieve a consistent model. The crystals were generally weakly diffracting and with the voids present in the structure this was the best final r-factor that could be achieved. 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^)+(0.1715P)^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_number_reflns 16197 _refine_ls_number_parameters 645 _refine_ls_number_restraints 836 _refine_ls_R_factor_all 0.1986 _refine_ls_R_factor_gt 0.1167 _refine_ls_wR_factor_ref 0.3640 _refine_ls_wR_factor_gt 0.3099 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.047 _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 0.38192(2) -0.34873(5) 0.37877(2) 0.0622(3) Uani 1 1 d . . . Ag2 Ag 0.29027(3) 0.37106(5) 0.13124(2) 0.0596(3) Uani 1 1 d . . . N111 N 0.40803(17) -0.5363(3) 0.38223(17) 0.0550(19) Uani 1 1 d GU . . C112 C 0.45166(16) -0.5482(4) 0.39568(16) 0.053(2) Uani 1 1 d GU . . C113 C 0.46987(15) -0.6588(5) 0.39546(19) 0.071(3) Uani 1 1 d GU . . H113 H 0.4997 -0.6669 0.4047 0.085 Uiso 1 1 calc R . . C114 C 0.4444(2) -0.7573(4) 0.3818(2) 0.076(3) Uani 1 1 d GU . . H114 H 0.4569 -0.8329 0.3817 0.091 Uiso 1 1 calc R . . C115 C 0.4008(2) -0.7454(4) 0.3684(2) 0.075(3) Uani 1 1 d GU . . H115 H 0.3834 -0.8127 0.3590 0.090 Uiso 1 1 calc R . . C116 C 0.38260(15) -0.6348(4) 0.36857(19) 0.066(3) Uani 1 1 d GU . . H116 H 0.3528 -0.6266 0.3594 0.079 Uiso 1 1 calc R . . N121 N 0.48865(19) -0.2509(4) 0.42065(17) 0.067(2) Uani 1 1 d GU . . N122 N 0.45666(14) -0.3351(5) 0.40331(15) 0.0529(18) Uani 1 1 d GU . . C123 C 0.4753(2) -0.4500(4) 0.40901(18) 0.0517(19) Uani 1 1 d GU . . C124 C 0.51879(19) -0.4369(6) 0.42989(19) 0.074(3) Uani 1 1 d GU . . H124 H 0.5389 -0.4994 0.4377 0.089 Uiso 1 1 calc R . . C125 C 0.52705(15) -0.3138(7) 0.43708(18) 0.078(3) Uani 1 1 d GU . . H125 H 0.5536 -0.2795 0.4505 0.094 Uiso 1 1 calc R . . C126 C 0.4801(4) -0.1312(9) 0.4171(3) 0.072(2) Uani 1 1 d U . . H12A H 0.5058 -0.0866 0.4313 0.087 Uiso 1 1 calc R . . H12B H 0.4580 -0.1129 0.4267 0.087 Uiso 1 1 calc R . . N131 N 0.31350(19) 0.5589(3) 0.12822(19) 0.059(2) Uani 1 1 d GU . . C132 C 0.3512(2) 0.5685(5) 0.1226(3) 0.078(3) Uani 1 1 d GU . . C133 C 0.3700(3) 0.6792(6) 0.1243(3) 0.118(5) Uani 1 1 d GU . . H133 H 0.3958 0.6857 0.1205 0.142 Uiso 1 1 calc R . . C134 C 0.3512(3) 0.7803(5) 0.1316(3) 0.134(6) Uani 1 1 d GU . . H134 H 0.3640 0.8559 0.1327 0.161 Uiso 1 1 calc R . . C135 C 0.3135(3) 0.7707(4) 0.1372(3) 0.103(4) Uani 1 1 d GU . . H135 H 0.3006 0.8398 0.1422 0.123 Uiso 1 1 calc R . . C136 C 0.2947(2) 0.6600(4) 0.1355(3) 0.077(3) Uani 1 1 d GU . . H136 H 0.2689 0.6534 0.1393 0.093 Uiso 1 1 calc R . . N141 N 0.3758(2) 0.2696(4) 0.1083(2) 0.078(3) Uani 1 1 d GU . . N142 N 0.35065(19) 0.3577(5) 0.1160(2) 0.057(2) Uani 1 1 d GU . . C143 C 0.3687(3) 0.4707(4) 0.1147(3) 0.077(3) Uani 1 1 d GU . . C144 C 0.4050(3) 0.4523(6) 0.1062(3) 0.110(5) Uani 1 1 d GU . . H144 H 0.4232 0.5126 0.1035 0.132 Uiso 1 1 calc R . . C145 C 0.4094(3) 0.3280(7) 0.1022(3) 0.119(5) Uani 1 1 d GU . . H145 H 0.4311 0.2906 0.0965 0.143 Uiso 1 1 calc R . . C146 C 0.3682(4) 0.1475(8) 0.1110(3) 0.076(3) Uani 1 1 d U . . H14A H 0.3836 0.1008 0.0991 0.091 Uiso 1 1 calc R . . H14B H 0.3377 0.1314 0.0988 0.091 Uiso 1 1 calc R . . C151 C 0.46546(9) -0.0902(4) 0.37913(9) 0.069(2) Uani 1 1 d GU A . C152 C 0.42442(9) -0.0545(2) 0.35959(8) 0.086(3) Uani 1 1 d GU . . H152 H 0.4041 -0.0506 0.3705 0.103 Uiso 1 1 calc R . . C153 C 0.41306(9) -0.02460(19) 0.32413(8) 0.091(3) Uani 1 1 d GU A . H153 H 0.3850 -0.0002 0.3108 0.109 Uiso 1 1 calc R . . C154 C 0.44274(10) -0.0304(2) 0.30822(9) 0.096(3) Uani 1 1 d GDU . . C155 C 0.48378(9) -0.0661(4) 0.32775(10) 0.097(3) Uani 1 1 d GU A . H155 H 0.5041 -0.0700 0.3169 0.116 Uiso 1 1 calc R . . C156 C 0.49514(9) -0.0960(4) 0.36321(10) 0.091(3) Uani 1 1 d GU . . H156 H 0.5232 -0.1204 0.3766 0.109 Uiso 1 1 calc R A . C161 C 0.38138(18) 0.1097(4) 0.14773(9) 0.067(2) Uani 1 1 d GU A . C162 C 0.35234(16) 0.0816(4) 0.16315(9) 0.073(3) Uani 1 1 d GU . . H162 H 0.3230 0.0843 0.1495 0.088 Uiso 1 1 calc R . . C163 C 0.36624(14) 0.0497(3) 0.19862(8) 0.089(3) Uani 1 1 d GU A . H163 H 0.3464 0.0305 0.2092 0.107 Uiso 1 1 calc R . . C164 C 0.40919(13) 0.0458(2) 0.21867(9) 0.092(3) Uani 1 1 d GU . . C165 C 0.43823(15) 0.0738(3) 0.20325(10) 0.099(3) Uani 1 1 d GU A . H165 H 0.4676 0.0711 0.2170 0.118 Uiso 1 1 calc R . . C166 C 0.42433(17) 0.1058(3) 0.16778(10) 0.091(3) Uani 1 1 d GU . . H166 H 0.4442 0.1249 0.1572 0.110 Uiso 1 1 calc R A . N171 N 0.40368(12) 0.0151(2) 0.25053(8) 0.073(5) Uani 0.421(16) 1 d PGU A 1 N172 N 0.44939(11) -0.0071(3) 0.27840(9) 0.066(4) Uani 0.421(16) 1 d PGDU A 1 N173 N 0.44031(12) 0.0169(2) 0.25596(9) 0.067(3) Uani 0.579(16) 1 d PGU A 2 N174 N 0.41236(11) 0.00734(19) 0.26834(9) 0.062(3) Uani 0.579(16) 1 d PGU A 2 N211 N 0.35225(12) -0.1933(3) 0.39986(10) 0.0594(19) Uani 1 1 d GU . . C212 C 0.32822(10) -0.1143(3) 0.37399(10) 0.0461(18) Uani 1 1 d GU . . C213 C 0.31169(12) -0.0127(4) 0.38351(10) 0.059(2) Uani 1 1 d GU . . H213 H 0.2953 0.0413 0.3658 0.071 Uiso 1 1 calc R . . C214 C 0.31920(14) 0.0099(4) 0.41891(11) 0.072(3) Uani 1 1 d GU . . H214 H 0.3079 0.0793 0.4254 0.087 Uiso 1 1 calc R . . C215 C 0.34323(14) -0.0692(4) 0.44478(10) 0.081(3) Uani 1 1 d GU . . H215 H 0.3484 -0.0537 0.4690 0.097 Uiso 1 1 calc R . . C216 C 0.35975(13) -0.1707(3) 0.43526(10) 0.073(3) Uani 1 1 d GU . . H216 H 0.3762 -0.2248 0.4529 0.087 Uiso 1 1 calc R . . N221 N 0.3280(2) -0.2482(4) 0.29345(15) 0.076(3) Uani 1 1 d GU . . N222 N 0.33921(19) -0.2452(4) 0.33070(14) 0.0561(19) Uani 1 1 d GU . . C223 C 0.3217(2) -0.1404(4) 0.33927(14) 0.054(2) Uani 1 1 d GU . . C224 C 0.2997(2) -0.0786(4) 0.30731(17) 0.076(3) Uani 1 1 d GU . . H224 H 0.2850 -0.0056 0.3052 0.091 Uiso 1 1 calc R . . C225 C 0.3035(3) -0.1453(5) 0.27899(13) 0.094(4) Uani 1 1 d GU . . H225 H 0.2918 -0.1246 0.2547 0.113 Uiso 1 1 calc R . . C226 C 0.3386(4) -0.3436(7) 0.2765(3) 0.086(3) Uani 1 1 d U . . H22A H 0.3157 -0.3558 0.2532 0.103 Uiso 1 1 calc R . . H22B H 0.3405 -0.4165 0.2907 0.103 Uiso 1 1 calc R . . C231 C 0.3792(3) -0.3284(6) 0.2708(3) 0.092(3) Uani 1 1 d GU . . C232 C 0.3792(3) -0.2893(6) 0.2384(2) 0.108(4) Uani 1 1 d GU . . H232 H 0.3534 -0.2687 0.2200 0.130 Uiso 1 1 calc R . . C233 C 0.4169(4) -0.2802(6) 0.2328(3) 0.130(4) Uani 1 1 d GU . . H233 H 0.4169 -0.2535 0.2107 0.156 Uiso 1 1 calc R . . C234 C 0.4547(3) -0.3103(7) 0.2597(4) 0.130(5) Uani 1 1 d GDU . . C235 C 0.4547(3) -0.3495(7) 0.2921(3) 0.126(4) Uani 1 1 d GU . . H235 H 0.4805 -0.3701 0.3105 0.151 Uiso 1 1 calc R . . C236 C 0.4170(4) -0.3586(6) 0.2977(2) 0.104(4) Uani 1 1 d GU . . H236 H 0.4170 -0.3853 0.3198 0.125 Uiso 1 1 calc R . . N241 N 0.5025(4) -0.3093(9) 0.2637(3) 0.131(5) Uani 1 1 d DU . . N311 N 0.24667(17) 0.2085(4) 0.10868(15) 0.0498(17) Uani 1 1 d GU . . C312 C 0.23941(19) 0.1377(4) 0.13387(12) 0.051(2) Uani 1 1 d GU . . C313 C 0.2153(2) 0.0348(4) 0.12359(15) 0.055(2) Uani 1 1 d GU . . H313 H 0.2104 -0.0136 0.1408 0.066 Uiso 1 1 calc R . . C314 C 0.1985(2) 0.0027(5) 0.08812(17) 0.072(3) Uani 1 1 d GU . . H314 H 0.1821 -0.0676 0.0811 0.087 Uiso 1 1 calc R . . C315 C 0.2058(2) 0.0735(6) 0.06292(13) 0.082(3) Uani 1 1 d GU . . H315 H 0.1943 0.0516 0.0387 0.099 Uiso 1 1 calc R . . C316 C 0.2299(2) 0.1764(5) 0.07320(14) 0.073(3) Uani 1 1 d GU . . H316 H 0.2348 0.2248 0.0560 0.087 Uiso 1 1 calc R . . N321 N 0.2958(2) 0.2839(4) 0.21551(14) 0.080(3) Uani 1 1 d GU . . N322 N 0.2799(2) 0.2763(4) 0.17804(14) 0.057(2) Uani 1 1 d GU . . C323 C 0.2559(2) 0.1700(4) 0.16804(12) 0.054(2) Uani 1 1 d GU . . C324 C 0.2570(3) 0.1118(4) 0.19933(15) 0.071(3) Uani 1 1 d GU . . H324 H 0.2436 0.0387 0.2004 0.085 Uiso 1 1 calc R . . C325 C 0.2816(3) 0.1822(5) 0.22867(12) 0.095(4) Uani 1 1 d GU . . H325 H 0.2876 0.1644 0.2529 0.114 Uiso 1 1 calc R . . C326 C 0.3165(5) 0.3834(8) 0.2320(3) 0.093(3) Uani 1 1 d U . . H32A H 0.3117 0.3958 0.2544 0.112 Uiso 1 1 calc R . . H32B H 0.3056 0.4537 0.2168 0.112 Uiso 1 1 calc R . . C331 C 0.3639(2) 0.3686(5) 0.23992(19) 0.079(3) Uani 1 1 d GU . . C332 C 0.3796(3) 0.4013(5) 0.21421(14) 0.085(3) Uani 1 1 d GU . . H332 H 0.3610 0.4304 0.1920 0.102 Uiso 1 1 calc R . . C333 C 0.4225(3) 0.3913(5) 0.22099(17) 0.084(3) Uani 1 1 d GU . . H333 H 0.4333 0.4136 0.2034 0.100 Uiso 1 1 calc R . . C334 C 0.4496(2) 0.3487(5) 0.2535(2) 0.083(3) Uani 1 1 d GU . . C335 C 0.4339(3) 0.3160(5) 0.27920(15) 0.099(3) Uani 1 1 d GU . . H335 H 0.4525 0.2869 0.3014 0.119 Uiso 1 1 calc R . . C336 C 0.3910(3) 0.3260(5) 0.27242(17) 0.098(3) Uani 1 1 d GU . . H336 H 0.3802 0.3037 0.2900 0.117 Uiso 1 1 calc R . . N341 N 0.4946(4) 0.3425(6) 0.2625(2) 0.087(3) Uani 1 1 d U . . B11 B 0.7635(3) 0.7763(7) 0.3157(2) 0.037(3) Uiso 0.596(13) 1 d PD B 1 F12 F 0.7262(2) 0.8384(5) 0.3106(2) 0.047(2) Uiso 0.596(13) 1 d PD B 1 B11X B 0.7839(3) 0.7445(8) 0.3174(2) 0.042(5) Uiso 0.404(13) 1 d PD B 2 F12X F 0.8200(3) 0.6887(8) 0.3173(3) 0.050(4) Uiso 0.404(13) 1 d PD B 2 F13 F 0.78569(16) 0.7599(4) 0.35129(13) 0.0579(12) Uiso 1 1 d D . . F14 F 0.74955(17) 0.6750(4) 0.29796(15) 0.0691(15) Uiso 1 1 d D . . F15 F 0.78616(18) 0.8474(4) 0.30112(16) 0.0706(15) Uiso 1 1 d D . . B21 B 0.5925(4) 1.0252(10) 0.9450(3) 0.095(5) Uiso 1 1 d D . . F22 F 0.5649(4) 0.9496(11) 0.9224(3) 0.207(5) Uiso 1 1 d D . . F23 F 0.5762(3) 1.0615(9) 0.9690(3) 0.151(3) Uiso 1 1 d D . . F24 F 0.6298(4) 0.9660(14) 0.9635(4) 0.266(8) Uiso 1 1 d D . . F25 F 0.6016(5) 1.1195(11) 0.9277(4) 0.205(6) Uiso 1 1 d D . . C11S C 0.5462(4) 0.7262(9) 0.9929(4) 0.087(7) Uiso 0.50 1 d PGU . . C12S C 0.5415(4) 0.6340(11) 1.0140(4) 0.070(5) Uiso 0.50 1 d PGU . . H12S H 0.5202 0.6383 1.0238 0.084 Uiso 0.50 1 calc PR . . C13S C 0.5679(5) 0.5354(10) 1.0206(4) 0.075(6) Uiso 0.50 1 d PGU . . H13S H 0.5647 0.4724 1.0350 0.091 Uiso 0.50 1 calc PR . . C14S C 0.5990(5) 0.5291(10) 1.0063(4) 0.084(6) Uiso 0.50 1 d PGU . . H14S H 0.6171 0.4618 1.0109 0.101 Uiso 0.50 1 calc PR . . C15S C 0.6038(5) 0.6213(12) 0.9853(4) 0.083(6) Uiso 0.50 1 d PGU . . H15S H 0.6250 0.6170 0.9755 0.100 Uiso 0.50 1 calc PR . . C16S C 0.5773(5) 0.7198(11) 0.9786(4) 0.083(6) Uiso 0.50 1 d PGU . . H16S H 0.5805 0.7828 0.9642 0.099 Uiso 0.50 1 calc PR . . C17S C 0.5140(6) 0.8384(13) 0.9868(6) 0.111(9) Uiso 0.50 1 d PGU . . H17A H 0.4873 0.8201 0.9675 0.167 Uiso 0.50 1 calc PR . . H17B H 0.5266 0.9093 0.9807 0.167 Uiso 0.50 1 calc PR . . H17C H 0.5086 0.8534 1.0085 0.167 Uiso 0.50 1 calc PR . . C23S C 0.2083(5) 0.2462(11) -0.0199(4) 0.095(4) Uiso 1 1 d DU . . C22S C 0.2255(5) 0.3500(10) -0.0047(4) 0.101(4) Uiso 1 1 d DU . . C21S C 0.2681(6) 0.3562(12) 0.0166(5) 0.103(4) Uiso 1 1 d U . . C24S C 0.2818(11) 0.455(3) 0.0317(10) 0.119(10) Uiso 0.50 1 d PU . . 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 0.0425(5) 0.0441(3) 0.0933(7) 0.0209(3) 0.0173(5) 0.0108(3) Ag2 0.0635(6) 0.0493(4) 0.0824(6) 0.0183(3) 0.0459(5) 0.0022(3) N111 0.051(4) 0.055(3) 0.064(6) 0.016(3) 0.028(4) 0.010(3) C112 0.059(5) 0.060(4) 0.049(6) 0.015(4) 0.028(5) 0.014(3) C113 0.062(6) 0.078(5) 0.081(8) 0.017(5) 0.037(6) 0.028(4) C114 0.078(6) 0.055(4) 0.110(9) 0.027(5) 0.054(7) 0.026(4) C115 0.075(6) 0.059(4) 0.105(9) 0.027(5) 0.049(7) 0.017(4) C116 0.067(6) 0.041(4) 0.100(8) 0.022(4) 0.045(6) 0.009(3) N121 0.038(5) 0.099(4) 0.059(6) -0.013(4) 0.013(4) -0.009(4) N122 0.046(4) 0.060(3) 0.048(5) -0.001(3) 0.013(4) -0.001(3) C123 0.035(4) 0.089(4) 0.033(5) 0.008(4) 0.015(4) 0.015(4) C124 0.038(5) 0.133(7) 0.051(7) -0.006(6) 0.015(5) 0.026(5) C125 0.031(5) 0.147(7) 0.054(7) -0.023(6) 0.014(5) -0.003(5) C126 0.057(7) 0.084(5) 0.084(6) -0.029(5) 0.035(6) -0.028(4) N131 0.067(5) 0.044(3) 0.083(6) 0.026(3) 0.048(5) 0.007(3) C132 0.086(8) 0.062(4) 0.116(9) 0.011(5) 0.074(8) -0.007(4) C133 0.123(11) 0.081(5) 0.212(15) -0.015(8) 0.132(11) -0.028(6) C134 0.162(12) 0.069(5) 0.244(16) -0.028(8) 0.159(13) -0.042(7) C135 0.129(10) 0.057(5) 0.172(13) -0.004(6) 0.114(10) -0.008(6) C136 0.078(8) 0.050(4) 0.123(10) 0.026(5) 0.061(8) 0.006(4) N141 0.077(7) 0.089(4) 0.088(7) -0.022(4) 0.053(6) -0.007(4) N142 0.047(5) 0.064(4) 0.067(6) -0.007(4) 0.030(5) 0.001(3) C143 0.083(8) 0.081(5) 0.095(9) -0.013(6) 0.065(7) -0.014(5) C144 0.118(10) 0.112(7) 0.154(12) -0.057(8) 0.114(10) -0.044(7) C145 0.107(10) 0.119(7) 0.177(14) -0.061(9) 0.106(11) -0.029(7) C146 0.064(7) 0.068(5) 0.080(6) -0.024(5) 0.009(6) 0.006(4) C151 0.083(6) 0.055(4) 0.076(6) -0.024(4) 0.037(5) -0.035(4) C152 0.075(6) 0.075(6) 0.104(7) -0.012(6) 0.029(6) -0.036(5) C153 0.111(8) 0.052(5) 0.097(7) -0.004(5) 0.022(6) -0.041(5) C154 0.143(9) 0.045(4) 0.092(6) -0.011(5) 0.031(6) -0.056(6) C155 0.129(8) 0.088(7) 0.079(7) -0.008(6) 0.044(6) -0.039(7) C156 0.089(8) 0.111(8) 0.079(7) -0.023(6) 0.039(6) -0.028(7) C161 0.063(6) 0.060(4) 0.073(6) -0.032(4) 0.019(5) 0.015(4) C162 0.061(6) 0.069(5) 0.085(6) -0.020(5) 0.022(5) 0.024(5) C163 0.117(8) 0.065(5) 0.085(7) 0.001(5) 0.037(6) 0.034(6) C164 0.132(9) 0.049(5) 0.073(6) -0.019(4) 0.013(5) 0.029(6) C165 0.099(8) 0.089(7) 0.086(7) -0.025(6) 0.008(6) 0.016(7) C166 0.059(6) 0.117(9) 0.087(7) -0.026(7) 0.014(6) 0.008(7) N171 0.061(11) 0.034(8) 0.110(8) -0.004(8) 0.015(7) 0.006(8) N172 0.054(10) 0.037(7) 0.097(9) 0.003(8) 0.016(7) -0.023(8) N173 0.047(8) 0.053(7) 0.092(7) -0.040(6) 0.017(6) 0.000(6) N174 0.061(9) 0.014(4) 0.118(7) 0.001(5) 0.039(7) 0.001(5) N211 0.037(5) 0.064(4) 0.070(5) 0.020(4) 0.011(4) -0.005(3) C212 0.038(5) 0.036(3) 0.061(5) 0.007(3) 0.013(4) -0.005(3) C213 0.063(7) 0.054(4) 0.063(6) 0.005(4) 0.026(6) 0.004(4) C214 0.071(8) 0.083(6) 0.063(6) -0.002(5) 0.025(6) 0.009(5) C215 0.064(8) 0.115(8) 0.067(7) 0.018(5) 0.028(6) 0.014(6) C216 0.061(7) 0.090(6) 0.070(6) 0.024(5) 0.029(6) 0.006(5) N221 0.100(7) 0.034(3) 0.056(5) -0.002(3) -0.015(5) 0.017(4) N222 0.052(5) 0.032(3) 0.068(5) 0.004(3) 0.003(4) 0.005(3) C223 0.055(6) 0.029(3) 0.063(5) -0.001(3) 0.004(5) -0.001(3) C224 0.094(8) 0.040(4) 0.057(5) -0.002(4) -0.015(6) 0.022(4) C225 0.121(11) 0.052(5) 0.056(6) -0.006(4) -0.030(7) 0.031(5) C226 0.100(7) 0.038(4) 0.069(7) -0.019(4) -0.027(6) 0.017(5) C231 0.109(7) 0.041(4) 0.093(8) -0.036(5) -0.001(6) 0.002(5) C232 0.140(9) 0.056(6) 0.096(8) -0.032(5) 0.006(8) 0.008(7) C233 0.181(11) 0.048(5) 0.162(12) -0.017(7) 0.063(9) -0.008(8) C234 0.151(9) 0.043(6) 0.188(13) -0.050(7) 0.052(10) -0.008(7) C235 0.103(8) 0.062(6) 0.184(12) -0.019(8) 0.021(9) -0.006(7) C236 0.106(8) 0.052(5) 0.119(9) -0.011(6) 0.001(7) 0.014(6) N241 0.192(10) 0.072(5) 0.136(15) -0.005(6) 0.067(12) 0.032(8) N311 0.044(5) 0.058(4) 0.060(4) 0.014(3) 0.034(4) 0.009(3) C312 0.066(6) 0.038(3) 0.060(5) 0.006(3) 0.036(5) 0.011(3) C313 0.049(6) 0.053(4) 0.066(5) 0.010(4) 0.024(5) 0.001(4) C314 0.078(8) 0.079(6) 0.069(6) -0.008(5) 0.038(6) -0.025(5) C315 0.072(8) 0.114(8) 0.058(6) 0.003(5) 0.022(6) -0.027(6) C316 0.067(8) 0.098(6) 0.067(6) 0.011(5) 0.042(6) -0.016(5) N321 0.162(8) 0.039(3) 0.070(5) -0.017(3) 0.079(6) -0.024(4) N322 0.091(6) 0.032(3) 0.071(5) -0.006(3) 0.056(5) -0.006(3) C323 0.082(7) 0.033(3) 0.064(4) 0.004(3) 0.047(5) 0.003(3) C324 0.136(10) 0.036(3) 0.051(5) -0.001(3) 0.047(6) -0.013(4) C325 0.196(13) 0.045(4) 0.067(6) -0.024(4) 0.076(8) -0.051(6) C326 0.181(8) 0.043(4) 0.084(7) -0.024(4) 0.082(7) -0.046(5) C331 0.170(8) 0.027(3) 0.060(6) -0.015(3) 0.066(6) -0.035(5) C332 0.146(8) 0.055(5) 0.059(6) -0.002(4) 0.044(7) -0.033(6) C333 0.142(8) 0.054(5) 0.064(6) 0.001(4) 0.048(7) -0.023(6) C334 0.164(8) 0.035(4) 0.056(6) -0.006(4) 0.049(6) -0.007(6) C335 0.189(9) 0.057(5) 0.058(7) -0.004(5) 0.053(7) -0.017(7) C336 0.201(9) 0.044(4) 0.074(7) 0.000(4) 0.081(7) -0.022(7) N341 0.166(8) 0.041(3) 0.050(6) 0.001(3) 0.035(7) 0.006(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 N111 2.272(4) . ? Ag1 N222 2.280(4) . ? Ag1 N211 2.334(4) . ? Ag1 N122 2.375(5) . ? Ag2 N131 2.273(4) . ? Ag2 N322 2.319(4) . ? Ag2 N311 2.320(4) . ? Ag2 N142 2.364(4) . ? N111 C112 1.3900 . ? N111 C116 1.3900 . ? C112 C123 1.356(7) . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C113 H113 0.9500 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C126 1.372(12) . ? N121 C125 1.4200 . ? N121 N122 1.4200 . ? N122 C123 1.4200 . ? C123 C124 1.4200 . ? C124 C125 1.4200 . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C151 1.512(13) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? N131 C132 1.3900 . ? N131 C136 1.3900 . ? C132 C143 1.345(6) . ? C132 C133 1.3900 . ? C133 C134 1.3900 . ? C133 H133 0.9500 . ? C134 C135 1.3900 . ? C134 H134 0.9500 . ? C135 C136 1.3900 . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 C146 1.407(11) . ? N141 C145 1.4200 . ? N141 N142 1.4200 . ? N142 C143 1.4200 . ? C143 C144 1.4200 . ? C144 C145 1.4200 . ? C144 H144 0.9500 . ? C145 H145 0.9500 . ? C146 C161 1.455(13) . ? C146 H14A 0.9900 . ? C146 H14B 0.9900 . ? C151 C152 1.3900 . ? C151 C156 1.3900 . ? C152 C153 1.3900 . ? C152 H152 0.9500 . ? C153 C154 1.3900 . ? C153 H153 0.9500 . ? C154 N172 1.3395 . ? C154 C155 1.3900 . ? C154 N174 1.6266 . ? C155 C156 1.3900 . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? C161 C162 1.3901 . ? C161 C166 1.3903 . ? C162 C163 1.3896 . ? C162 H162 0.9500 . ? C163 C164 1.3902 . ? C163 H163 0.9500 . ? C164 C165 1.3899 . ? C164 N171 1.4189 . ? C164 N173 1.5317 . ? C165 C166 1.3901 . ? C165 H165 0.9500 . ? C166 H166 0.9500 . ? N171 N172 1.5735 . ? N173 N174 1.2360 . ? N211 C212 1.3900 . ? N211 C216 1.3900 . ? C212 C223 1.378(6) . ? C212 C213 1.3900 . ? C213 C214 1.3899 . ? C213 H213 0.9500 . ? C214 C215 1.3900 . ? C214 H214 0.9500 . ? C215 C216 1.3900 . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 C226 1.394(11) . ? N221 N222 1.4200 . ? N221 C225 1.4200 . ? N222 C223 1.4200 . ? C223 C224 1.4200 . ? C224 C225 1.4200 . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C226 C231 1.495(16) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? C231 C232 1.3900 . ? C231 C236 1.3900 . ? C232 C233 1.3900 . ? C232 H232 0.9500 . ? C233 C234 1.3900 . ? C233 H233 0.9500 . ? C234 C235 1.3900 . ? C234 N241 1.579(9) . ? C235 C236 1.3900 . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? N241 N241 1.06(2) 2_655 ? N311 C312 1.3900 . ? N311 C316 1.3900 . ? C312 C323 1.343(6) . ? C312 C313 1.3900 . ? C313 C314 1.3900 . ? C313 H313 0.9500 . ? C314 C315 1.3900 . ? C314 H314 0.9500 . ? C315 C316 1.3900 . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N321 C326 1.360(10) . ? N321 C325 1.4200 . ? N321 N322 1.4200 . ? N322 C323 1.4200 . ? C323 C324 1.4200 . ? C324 C325 1.4200 . ? C324 H324 0.9500 . ? C325 H325 0.9500 . ? C326 C331 1.536(17) . ? C326 H32A 0.9900 . ? C326 H32B 0.9900 . ? C331 C332 1.3900 . ? C331 C336 1.3900 . ? C332 C333 1.3900 . ? C332 H332 0.9500 . ? C333 C334 1.3900 . ? C333 H333 0.9500 . ? C334 C335 1.3900 . ? C334 N341 1.440(15) . ? C335 C336 1.3900 . ? C335 H335 0.9500 . ? C336 H336 0.9500 . ? N341 N341 1.201(18) 2_655 ? B11 F14 1.338(8) . ? B11 F13 1.376(8) . ? B11 F15 1.390(8) . ? B11 F12 1.395(8) . ? B11X F15 1.348(9) . ? B11X F13 1.369(9) . ? B11X F12X 1.382(9) . ? B11X F14 1.388(9) . ? B21 F22 1.346(9) . ? B21 F23 1.352(9) . ? B21 F25 1.369(9) . ? B21 F24 1.387(9) . ? C11S C12S 1.3900 . ? C11S C16S 1.3900 . ? C11S C17S 1.6299 . ? C12S C13S 1.3900 . ? C12S H12S 0.9500 . ? C13S C14S 1.3900 . ? C13S H13S 0.9500 . ? C14S C15S 1.3900 . ? C14S H14S 0.9500 . ? C15S C16S 1.3900 . ? C15S H15S 0.9500 . ? C16S H16S 0.9500 . ? C17S H17A 0.9800 . ? C17S H17B 0.9800 . ? C17S H17C 0.9800 . ? C23S C22S 1.348(9) . ? C23S C21S 1.382(18) 7 ? C22S C21S 1.39(2) . ? C21S C24S 1.27(3) . ? C21S C23S 1.382(18) 7 ? 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 N111 Ag1 N222 129.7(2) . . ? N111 Ag1 N211 152.15(17) . . ? N222 Ag1 N211 72.98(16) . . ? N111 Ag1 N122 72.44(19) . . ? N222 Ag1 N122 125.1(2) . . ? N211 Ag1 N122 109.93(16) . . ? N131 Ag2 N322 129.2(2) . . ? N131 Ag2 N311 153.5(2) . . ? N322 Ag2 N311 72.19(18) . . ? N131 Ag2 N142 71.95(18) . . ? N322 Ag2 N142 126.6(2) . . ? N311 Ag2 N142 109.87(19) . . ? C112 N111 C116 120.0 . . ? C112 N111 Ag1 116.9(3) . . ? C116 N111 Ag1 122.8(3) . . ? C123 C112 N111 118.1(4) . . ? C123 C112 C113 121.9(4) . . ? N111 C112 C113 120.0 . . ? C112 C113 C114 120.0 . . ? C112 C113 H113 120.0 . . ? C114 C113 H113 120.0 . . ? C115 C114 C113 120.0 . . ? C115 C114 H114 120.0 . . ? C113 C114 H114 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H115 120.0 . . ? C116 C115 H115 120.0 . . ? C115 C116 N111 120.0 . . ? C115 C116 H116 120.0 . . ? N111 C116 H116 120.0 . . ? C126 N121 C125 131.3(6) . . ? C126 N121 N122 120.4(7) . . ? C125 N121 N122 108.0 . . ? N121 N122 C123 108.0 . . ? N121 N122 Ag1 139.5(3) . . ? C123 N122 Ag1 110.9(3) . . ? C112 C123 C124 131.3(5) . . ? C112 C123 N122 120.7(5) . . ? C124 C123 N122 108.0 . . ? C123 C124 C125 108.0 . . ? C123 C124 H124 126.0 . . ? C125 C124 H124 126.0 . . ? N121 C125 C124 108.0 . . ? N121 C125 H125 126.0 . . ? C124 C125 H125 126.0 . . ? N121 C126 C151 112.5(8) . . ? N121 C126 H12A 109.1 . . ? C151 C126 H12A 109.1 . . ? N121 C126 H12B 109.1 . . ? C151 C126 H12B 109.1 . . ? H12A C126 H12B 107.8 . . ? C132 N131 C136 120.0 . . ? C132 N131 Ag2 116.3(3) . . ? C136 N131 Ag2 123.3(3) . . ? C143 C132 C133 120.3(5) . . ? C143 C132 N131 119.6(5) . . ? C133 C132 N131 120.0 . . ? C132 C133 C134 120.0 . . ? C132 C133 H133 120.0 . . ? C134 C133 H133 120.0 . . ? C135 C134 C133 120.0 . . ? C135 C134 H134 120.0 . . ? C133 C134 H134 120.0 . . ? C134 C135 C136 120.0 . . ? C134 C135 H135 120.0 . . ? C136 C135 H135 120.0 . . ? C135 C136 N131 120.0 . . ? C135 C136 H136 120.0 . . ? N131 C136 H136 120.0 . . ? C146 N141 C145 130.5(7) . . ? C146 N141 N142 121.1(7) . . ? C145 N141 N142 108.0 . . ? N141 N142 C143 108.0 . . ? N141 N142 Ag2 139.4(3) . . ? C143 N142 Ag2 112.6(3) . . ? C132 C143 C144 133.0(5) . . ? C132 C143 N142 119.0(5) . . ? C144 C143 N142 108.0 . . ? C145 C144 C143 108.0 . . ? C145 C144 H144 126.0 . . ? C143 C144 H144 126.0 . . ? N141 C145 C144 108.0 . . ? N141 C145 H145 126.0 . . ? C144 C145 H145 126.0 . . ? N141 C146 C161 111.7(8) . . ? N141 C146 H14A 109.3 . . ? C161 C146 H14A 109.3 . . ? N141 C146 H14B 109.3 . . ? C161 C146 H14B 109.3 . . ? H14A C146 H14B 108.0 . . ? C152 C151 C156 120.0 . . ? C152 C151 C126 123.8(4) . . ? C156 C151 C126 116.1(4) . . ? C151 C152 C153 120.0 . . ? C151 C152 H152 120.0 . . ? C153 C152 H152 120.0 . . ? C154 C153 C152 120.0 . . ? C154 C153 H153 120.0 . . ? C152 C153 H153 120.0 . . ? N172 C154 C155 95.9 . . ? N172 C154 C153 144.0 . . ? C155 C154 C153 120.0 . . ? N172 C154 N174 45.9 . . ? C155 C154 N174 141.5 . . ? C153 C154 N174 98.4 . . ? C156 C155 C154 120.0 . . ? C156 C155 H155 120.0 . . ? C154 C155 H155 120.0 . . ? C155 C156 C151 120.0 . . ? C155 C156 H156 120.0 . . ? C151 C156 H156 120.0 . . ? C162 C161 C166 120.0 . . ? C162 C161 C146 121.8(6) . . ? C166 C161 C146 118.2(6) . . ? C163 C162 C161 120.0 . . ? C163 C162 H162 120.0 . . ? C161 C162 H162 120.0 . . ? C162 C163 C164 120.0 . . ? C162 C163 H163 120.0 . . ? C164 C163 H163 120.0 . . ? C165 C164 C163 120.0 . . ? C165 C164 N171 145.5 . . ? C163 C164 N171 94.5 . . ? C165 C164 N173 98.4 . . ? C163 C164 N173 141.6 . . ? N171 C164 N173 47.2 . . ? C164 C165 C166 120.0 . . ? C164 C165 H165 120.0 . . ? C166 C165 H165 120.0 . . ? C165 C166 C161 120.0 . . ? C165 C166 H166 120.0 . . ? C161 C166 H166 120.0 . . ? C164 N171 N172 105.5 . . ? C154 N172 N171 103.3 . . ? N174 N173 C164 93.7 . . ? N173 N174 C154 97.2 . . ? C212 N211 C216 120.0 . . ? C212 N211 Ag1 114.45(10) . . ? C216 N211 Ag1 125.32(10) . . ? C223 C212 N211 117.9(3) . . ? C223 C212 C213 122.1(3) . . ? N211 C212 C213 120.0 . . ? C214 C213 C212 120.0 . . ? C214 C213 H213 120.0 . . ? C212 C213 H213 120.0 . . ? C213 C214 C215 120.0 . . ? C213 C214 H214 120.0 . . ? C215 C214 H214 120.0 . . ? C216 C215 C214 120.0 . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C215 C216 N211 120.0 . . ? C215 C216 H216 120.0 . . ? N211 C216 H216 120.0 . . ? C226 N221 N222 122.0(6) . . ? C226 N221 C225 129.9(6) . . ? N222 N221 C225 108.0 . . ? N221 N222 C223 108.0 . . ? N221 N222 Ag1 137.7(3) . . ? C223 N222 Ag1 113.9(3) . . ? C212 C223 C224 131.7(4) . . ? C212 C223 N222 120.3(4) . . ? C224 C223 N222 108.0 . . ? C225 C224 C223 108.0 . . ? C225 C224 H224 126.0 . . ? C223 C224 H224 126.0 . . ? C224 C225 N221 108.0 . . ? C224 C225 H225 126.0 . . ? N221 C225 H225 126.0 . . ? N221 C226 C231 114.5(8) . . ? N221 C226 H22A 108.6 . . ? C231 C226 H22A 108.6 . . ? N221 C226 H22B 108.6 . . ? C231 C226 H22B 108.6 . . ? H22A C226 H22B 107.6 . . ? C232 C231 C236 120.0 . . ? C232 C231 C226 120.4(9) . . ? C236 C231 C226 119.5(9) . . ? C231 C232 C233 120.0 . . ? C231 C232 H232 120.0 . . ? C233 C232 H232 120.0 . . ? C232 C233 C234 120.0 . . ? C232 C233 H233 120.0 . . ? C234 C233 H233 120.0 . . ? C235 C234 C233 120.0 . . ? C235 C234 N241 105.4(10) . . ? C233 C234 N241 134.5(10) . . ? C234 C235 C236 120.0 . . ? C234 C235 H235 120.0 . . ? C236 C235 H235 120.0 . . ? C235 C236 C231 120.0 . . ? C235 C236 H236 120.0 . . ? C231 C236 H236 120.0 . . ? N241 N241 C234 97.6(15) 2_655 . ? C312 N311 C316 120.0 . . ? C312 N311 Ag2 114.9(3) . . ? C316 N311 Ag2 125.0(3) . . ? C323 C312 N311 119.2(4) . . ? C323 C312 C313 120.8(4) . . ? N311 C312 C313 120.0 . . ? C314 C313 C312 120.0 . . ? C314 C313 H313 120.0 . . ? C312 C313 H313 120.0 . . ? C313 C314 C315 120.0 . . ? C313 C314 H314 120.0 . . ? C315 C314 H314 120.0 . . ? C316 C315 C314 120.0 . . ? C316 C315 H315 120.0 . . ? C314 C315 H315 120.0 . . ? C315 C316 N311 120.0 . . ? C315 C316 H316 120.0 . . ? N311 C316 H316 120.0 . . ? C326 N321 C325 131.4(6) . . ? C326 N321 N322 120.2(6) . . ? C325 N321 N322 108.0 . . ? C323 N322 N321 108.0 . . ? C323 N322 Ag2 113.4(3) . . ? N321 N322 Ag2 137.8(3) . . ? C312 C323 N322 120.1(4) . . ? C312 C323 C324 131.7(4) . . ? N322 C323 C324 108.0 . . ? C325 C324 C323 108.0 . . ? C325 C324 H324 126.0 . . ? C323 C324 H324 126.0 . . ? N321 C325 C324 108.0 . . ? N321 C325 H325 126.0 . . ? C324 C325 H325 126.0 . . ? N321 C326 C331 109.2(8) . . ? N321 C326 H32A 109.8 . . ? C331 C326 H32A 109.8 . . ? N321 C326 H32B 109.8 . . ? C331 C326 H32B 109.8 . . ? H32A C326 H32B 108.3 . . ? C332 C331 C336 120.0 . . ? C332 C331 C326 118.9(7) . . ? C336 C331 C326 121.1(7) . . ? C333 C332 C331 120.0 . . ? C333 C332 H332 120.0 . . ? C331 C332 H332 120.0 . . ? C334 C333 C332 120.0 . . ? C334 C333 H333 120.0 . . ? C332 C333 H333 120.0 . . ? C333 C334 C335 120.0 . . ? C333 C334 N341 122.1(6) . . ? C335 C334 N341 117.8(6) . . ? C336 C335 C334 120.0 . . ? C336 C335 H335 120.0 . . ? C334 C335 H335 120.0 . . ? C335 C336 C331 120.0 . . ? C335 C336 H336 120.0 . . ? C331 C336 H336 120.0 . . ? N341 N341 C334 114.6(15) 2_655 . ? F14 B11 F13 113.8(6) . . ? F14 B11 F15 113.6(7) . . ? F13 B11 F15 110.4(6) . . ? F14 B11 F12 102.8(6) . . ? F13 B11 F12 110.1(7) . . ? F15 B11 F12 105.5(6) . . ? F15 B11X F13 113.4(7) . . ? F15 B11X F12X 100.2(7) . . ? F13 B11X F12X 110.6(8) . . ? F15 B11X F14 113.1(7) . . ? F13 B11X F14 111.0(7) . . ? F12X B11X F14 108.0(8) . . ? B11X F13 B11 32.4(6) . . ? B11 F14 B11X 32.5(6) . . ? B11X F15 B11 32.4(6) . . ? F22 B21 F23 108.1(9) . . ? F22 B21 F25 111.9(10) . . ? F23 B21 F25 111.7(9) . . ? F22 B21 F24 109.8(10) . . ? F23 B21 F24 107.0(9) . . ? F25 B21 F24 108.3(9) . . ? C12S C11S C16S 120.0 . . ? C12S C11S C17S 116.5 . . ? C16S C11S C17S 123.5 . . ? C13S C12S C11S 120.0 . . ? C13S C12S H12S 120.0 . . ? C11S C12S H12S 120.0 . . ? C12S C13S C14S 120.0 . . ? C12S C13S H13S 120.0 . . ? C14S C13S H13S 120.0 . . ? C15S C14S C13S 120.0 . . ? C15S C14S H14S 120.0 . . ? C13S C14S H14S 120.0 . . ? C14S C15S C16S 120.0 . . ? C14S C15S H15S 120.0 . . ? C16S C15S H15S 120.0 . . ? C15S C16S C11S 120.0 . . ? C15S C16S H16S 120.0 . . ? C11S C16S H16S 120.0 . . ? C11S C17S H17A 109.5 . . ? C11S C17S H17B 109.5 . . ? H17A C17S H17B 109.5 . . ? C11S C17S H17C 109.5 . . ? H17A C17S H17C 109.5 . . ? H17B C17S H17C 109.5 . . ? C22S C23S C21S 122.4(14) . 7 ? C23S C22S C21S 120.5(13) . . ? C24S C21S C23S 126(2) . 7 ? C24S C21S C22S 117(2) . . ? C23S C21S C22S 117.0(13) 7 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N222 Ag1 N111 C112 120.7(4) . . . . ? N211 Ag1 N111 C112 -100.2(4) . . . . ? N122 Ag1 N111 C112 -0.7(3) . . . . ? N222 Ag1 N111 C116 -53.0(4) . . . . ? N211 Ag1 N111 C116 86.0(5) . . . . ? N122 Ag1 N111 C116 -174.4(4) . . . . ? C116 N111 C112 C123 -179.5(6) . . . . ? Ag1 N111 C112 C123 6.6(6) . . . . ? C116 N111 C112 C113 0.0 . . . . ? Ag1 N111 C112 C113 -173.9(4) . . . . ? C123 C112 C113 C114 179.4(6) . . . . ? N111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 N111 0.0 . . . . ? C112 N111 C116 C115 0.0 . . . . ? Ag1 N111 C116 C115 173.6(4) . . . . ? C126 N121 N122 C123 174.9(8) . . . . ? C125 N121 N122 C123 0.0 . . . . ? C126 N121 N122 Ag1 -21.7(9) . . . . ? C125 N121 N122 Ag1 163.4(6) . . . . ? N111 Ag1 N122 N121 -167.9(6) . . . . ? N222 Ag1 N122 N121 65.5(6) . . . . ? N211 Ag1 N122 N121 -17.2(6) . . . . ? N111 Ag1 N122 C123 -4.8(3) . . . . ? N222 Ag1 N122 C123 -131.4(3) . . . . ? N211 Ag1 N122 C123 145.9(3) . . . . ? N111 C112 C123 C124 167.0(5) . . . . ? C113 C112 C123 C124 -12.4(8) . . . . ? N111 C112 C123 N122 -11.9(7) . . . . ? C113 C112 C123 N122 168.7(4) . . . . ? N121 N122 C123 C112 179.1(7) . . . . ? Ag1 N122 C123 C112 10.6(6) . . . . ? N121 N122 C123 C124 0.0 . . . . ? Ag1 N122 C123 C124 -168.6(4) . . . . ? C112 C123 C124 C125 -179.0(7) . . . . ? N122 C123 C124 C125 0.0 . . . . ? C126 N121 C125 C124 -174.1(9) . . . . ? N122 N121 C125 C124 0.0 . . . . ? C123 C124 C125 N121 0.0 . . . . ? C125 N121 C126 C151 113.8(8) . . . . ? N122 N121 C126 C151 -59.7(9) . . . . ? N322 Ag2 N131 C132 117.5(5) . . . . ? N311 Ag2 N131 C132 -104.0(5) . . . . ? N142 Ag2 N131 C132 -5.5(5) . . . . ? N322 Ag2 N131 C136 -55.2(6) . . . . ? N311 Ag2 N131 C136 83.4(6) . . . . ? N142 Ag2 N131 C136 -178.2(5) . . . . ? C136 N131 C132 C143 -178.4(9) . . . . ? Ag2 N131 C132 C143 8.7(9) . . . . ? C136 N131 C132 C133 0.0 . . . . ? Ag2 N131 C132 C133 -172.9(5) . . . . ? C143 C132 C133 C134 178.4(10) . . . . ? N131 C132 C133 C134 0.0 . . . . ? C132 C133 C134 C135 0.0 . . . . ? C133 C134 C135 C136 0.0 . . . . ? C134 C135 C136 N131 0.0 . . . . ? C132 N131 C136 C135 0.0 . . . . ? Ag2 N131 C136 C135 172.4(6) . . . . ? C146 N141 N142 C143 173.8(10) . . . . ? C145 N141 N142 C143 0.0 . . . . ? C146 N141 N142 Ag2 -4.5(13) . . . . ? C145 N141 N142 Ag2 -178.3(9) . . . . ? N131 Ag2 N142 N141 -179.6(8) . . . . ? N322 Ag2 N142 N141 54.5(8) . . . . ? N311 Ag2 N142 N141 -27.6(8) . . . . ? N131 Ag2 N142 C143 2.2(5) . . . . ? N322 Ag2 N142 C143 -123.7(5) . . . . ? N311 Ag2 N142 C143 154.1(5) . . . . ? C133 C132 C143 C144 -1.6(12) . . . . ? N131 C132 C143 C144 176.7(7) . . . . ? C133 C132 C143 N142 174.9(6) . . . . ? N131 C132 C143 N142 -6.8(12) . . . . ? N141 N142 C143 C132 -177.3(10) . . . . ? Ag2 N142 C143 C132 1.5(9) . . . . ? N141 N142 C143 C144 0.0 . . . . ? Ag2 N142 C143 C144 178.8(6) . . . . ? C132 C143 C144 C145 176.8(12) . . . . ? N142 C143 C144 C145 0.0 . . . . ? C146 N141 C145 C144 -173.0(11) . . . . ? N142 N141 C145 C144 0.0 . . . . ? C143 C144 C145 N141 0.0 . . . . ? C145 N141 C146 C161 99.0(10) . . . . ? N142 N141 C146 C161 -73.2(11) . . . . ? N121 C126 C151 C152 109.8(7) . . . . ? N121 C126 C151 C156 -66.6(8) . . . . ? C156 C151 C152 C153 0.0 . . . . ? C126 C151 C152 C153 -176.3(5) . . . . ? C151 C152 C153 C154 0.0 . . . . ? C152 C153 C154 N172 -174.5 . . . . ? C152 C153 C154 C155 0.0 . . . . ? C152 C153 C154 N174 177.8 . . . . ? N172 C154 C155 C156 176.8 . . . . ? C153 C154 C155 C156 0.0 . . . . ? N174 C154 C155 C156 -176.6 . . . . ? C154 C155 C156 C151 0.0 . . . . ? C152 C151 C156 C155 0.0 . . . . ? C126 C151 C156 C155 176.6(5) . . . . ? N141 C146 C161 C162 108.1(8) . . . . ? N141 C146 C161 C166 -69.8(9) . . . . ? C166 C161 C162 C163 0.0 . . . . ? C146 C161 C162 C163 -177.8(5) . . . . ? C161 C162 C163 C164 0.0 . . . . ? C162 C163 C164 C165 0.0 . . . . ? C162 C163 C164 N171 177.7 . . . . ? C162 C163 C164 N173 -178.8 . . . . ? C163 C164 C165 C166 0.0 . . . . ? N171 C164 C165 C166 -175.9 . . . . ? N173 C164 C165 C166 179.2 . . . . ? C164 C165 C166 C161 0.0 . . . . ? C162 C161 C166 C165 0.0 . . . . ? C146 C161 C166 C165 177.9(5) . . . . ? C165 C164 N171 N172 -8.6 . . . . ? C163 C164 N171 N172 175.0 . . . . ? N173 C164 N171 N172 -2.0 . . . . ? C155 C154 N172 N171 170.9 . . . . ? C153 C154 N172 N171 -13.9 . . . . ? N174 C154 N172 N171 -3.3 . . . . ? C164 N171 N172 C154 177.3 . . . . ? C165 C164 N173 N174 172.6 . . . . ? C163 C164 N173 N174 -8.4 . . . . ? N171 C164 N173 N174 -3.6 . . . . ? C164 N173 N174 C154 177.3 . . . . ? N172 C154 N174 N173 -2.1 . . . . ? C155 C154 N174 N173 -11.4 . . . . ? C153 C154 N174 N173 171.6 . . . . ? N111 Ag1 N211 C212 -153.8(3) . . . . ? N222 Ag1 N211 C212 -5.70(18) . . . . ? N122 Ag1 N211 C212 116.20(18) . . . . ? N111 Ag1 N211 C216 31.7(4) . . . . ? N222 Ag1 N211 C216 179.82(18) . . . . ? N122 Ag1 N211 C216 -58.28(16) . . . . ? C216 N211 C212 C223 179.8(4) . . . . ? Ag1 N211 C212 C223 5.0(4) . . . . ? C216 N211 C212 C213 0.0 . . . . ? Ag1 N211 C212 C213 -174.80(11) . . . . ? C223 C212 C213 C214 -179.8(4) . . . . ? N211 C212 C213 C214 0.0 . . . . ? C212 C213 C214 C215 0.0 . . . . ? C213 C214 C215 C216 0.0 . . . . ? C214 C215 C216 N211 0.0 . . . . ? C212 N211 C216 C215 0.0 . . . . ? Ag1 N211 C216 C215 174.19(12) . . . . ? C226 N221 N222 C223 -176.7(10) . . . . ? C225 N221 N222 C223 0.0 . . . . ? C226 N221 N222 Ag1 11.5(11) . . . . ? C225 N221 N222 Ag1 -171.8(6) . . . . ? N111 Ag1 N222 N221 -21.6(7) . . . . ? N211 Ag1 N222 N221 177.1(6) . . . . ? N122 Ag1 N222 N221 74.3(6) . . . . ? N111 Ag1 N222 C223 167.0(3) . . . . ? N211 Ag1 N222 C223 5.6(3) . . . . ? N122 Ag1 N222 C223 -97.1(4) . . . . ? N211 C212 C223 C224 -179.0(5) . . . . ? C213 C212 C223 C224 0.8(7) . . . . ? N211 C212 C223 N222 0.2(6) . . . . ? C213 C212 C223 N222 180.0(3) . . . . ? N221 N222 C223 C212 -179.4(7) . . . . ? Ag1 N222 C223 C212 -5.4(6) . . . . ? N221 N222 C223 C224 0.0 . . . . ? Ag1 N222 C223 C224 174.0(5) . . . . ? C212 C223 C224 C225 179.2(8) . . . . ? N222 C223 C224 C225 0.0 . . . . ? C223 C224 C225 N221 0.0 . . . . ? C226 N221 C225 C224 176.4(11) . . . . ? N222 N221 C225 C224 0.0 . . . . ? N222 N221 C226 C231 -93.1(11) . . . . ? C225 N221 C226 C231 91.0(11) . . . . ? N221 C226 C231 C232 -97.9(9) . . . . ? N221 C226 C231 C236 84.8(9) . . . . ? C236 C231 C232 C233 0.0 . . . . ? C226 C231 C232 C233 -177.3(6) . . . . ? C231 C232 C233 C234 0.0 . . . . ? C232 C233 C234 C235 0.0 . . . . ? C232 C233 C234 N241 -178.5(9) . . . . ? C233 C234 C235 C236 0.0 . . . . ? N241 C234 C235 C236 178.9(6) . . . . ? C234 C235 C236 C231 0.0 . . . . ? C232 C231 C236 C235 0.0 . . . . ? C226 C231 C236 C235 177.3(6) . . . . ? C235 C234 N241 N241 160.9(3) . . . 2_655 ? C233 C234 N241 N241 -20.5(7) . . . 2_655 ? N131 Ag2 N311 C312 -151.1(4) . . . . ? N322 Ag2 N311 C312 -3.7(3) . . . . ? N142 Ag2 N311 C312 119.7(3) . . . . ? N131 Ag2 N311 C316 32.0(6) . . . . ? N322 Ag2 N311 C316 179.4(4) . . . . ? N142 Ag2 N311 C316 -57.2(4) . . . . ? C316 N311 C312 C323 179.9(6) . . . . ? Ag2 N311 C312 C323 2.8(6) . . . . ? C316 N311 C312 C313 0.0 . . . . ? Ag2 N311 C312 C313 -177.1(3) . . . . ? C323 C312 C313 C314 -179.9(6) . . . . ? N311 C312 C313 C314 0.0 . . . . ? C312 C313 C314 C315 0.0 . . . . ? C313 C314 C315 C316 0.0 . . . . ? C314 C315 C316 N311 0.0 . . . . ? C312 N311 C316 C315 0.0 . . . . ? Ag2 N311 C316 C315 176.7(4) . . . . ? C326 N321 N322 C323 -173.5(9) . . . . ? C325 N321 N322 C323 0.0 . . . . ? C326 N321 N322 Ag2 17.9(11) . . . . ? C325 N321 N322 Ag2 -168.6(6) . . . . ? N131 Ag2 N322 C323 166.0(3) . . . . ? N311 Ag2 N322 C323 4.1(3) . . . . ? N142 Ag2 N322 C323 -97.8(4) . . . . ? N131 Ag2 N322 N321 -25.9(6) . . . . ? N311 Ag2 N322 N321 172.2(6) . . . . ? N142 Ag2 N322 N321 70.3(6) . . . . ? N311 C312 C323 N322 1.1(7) . . . . ? C313 C312 C323 N322 -179.1(4) . . . . ? N311 C312 C323 C324 -173.9(5) . . . . ? C313 C312 C323 C324 6.0(8) . . . . ? N321 N322 C323 C312 -176.0(7) . . . . ? Ag2 N322 C323 C312 -4.3(6) . . . . ? N321 N322 C323 C324 0.0 . . . . ? Ag2 N322 C323 C324 171.7(5) . . . . ? C312 C323 C324 C325 175.4(8) . . . . ? N322 C323 C324 C325 0.0 . . . . ? C326 N321 C325 C324 172.5(11) . . . . ? N322 N321 C325 C324 0.0 . . . . ? C323 C324 C325 N321 0.0 . . . . ? C325 N321 C326 C331 97.8(9) . . . . ? N322 N321 C326 C331 -90.5(10) . . . . ? N321 C326 C331 C332 87.2(8) . . . . ? N321 C326 C331 C336 -94.3(8) . . . . ? C336 C331 C332 C333 0.0 . . . . ? C326 C331 C332 C333 178.5(6) . . . . ? C331 C332 C333 C334 0.0 . . . . ? C332 C333 C334 C335 0.0 . . . . ? C332 C333 C334 N341 -176.8(6) . . . . ? C333 C334 C335 C336 0.0 . . . . ? N341 C334 C335 C336 176.9(6) . . . . ? C334 C335 C336 C331 0.0 . . . . ? C332 C331 C336 C335 0.0 . . . . ? C326 C331 C336 C335 -178.5(6) . . . . ? C333 C334 N341 N341 -20.8(6) . . . 2_655 ? C335 C334 N341 N341 162.3(3) . . . 2_655 ? F15 B11X F13 B11 67.7(9) . . . . ? F12X B11X F13 B11 179.2(13) . . . . ? F14 B11X F13 B11 -60.9(9) . . . . ? F14 B11 F13 B11X 67.6(9) . . . . ? F15 B11 F13 B11X -61.5(9) . . . . ? F12 B11 F13 B11X -177.6(12) . . . . ? F13 B11 F14 B11X -65.2(9) . . . . ? F15 B11 F14 B11X 62.2(9) . . . . ? F12 B11 F14 B11X 175.8(12) . . . . ? F15 B11X F14 B11 -65.3(10) . . . . ? F13 B11X F14 B11 63.4(9) . . . . ? F12X B11X F14 B11 -175.2(13) . . . . ? F13 B11X F15 B11 -66.2(9) . . . . ? F12X B11X F15 B11 176.1(13) . . . . ? F14 B11X F15 B11 61.4(9) . . . . ? F14 B11 F15 B11X -66.1(9) . . . . ? F13 B11 F15 B11X 63.1(9) . . . . ? F12 B11 F15 B11X -178.0(12) . . . . ? C16S C11S C12S C13S 0.0 . . . . ? C17S C11S C12S C13S -179.6 . . . . ? C11S C12S C13S C14S 0.0 . . . . ? C12S C13S C14S C15S 0.0 . . . . ? C13S C14S C15S C16S 0.0 . . . . ? C14S C15S C16S C11S 0.0 . . . . ? C12S C11S C16S C15S 0.0 . . . . ? C17S C11S C16S C15S 179.5 . . . . ? C21S C23S C22S C21S -3(3) 7 . . . ? C23S C22S C21S C24S -176(2) . . . . ? C23S C22S C21S C23S 3(3) . . . 7 ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.68 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.379 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.144 data_2012ncs0335 _database_code_depnum_ccdc_archive 'CCDC 895603' #TrackingRef 'Ag_Ward_Stephenson_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C31 H24 Ag N6 O) 2(P F6)' _chemical_formula_sum 'C62 H48 Ag2 F12 N12 O2 P2' _chemical_formula_weight 1498.80 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6322 _symmetry_space_group_name_Hall 'P 6c 2c' _symmetry_Int_Tables_number 182 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' '-y, x-y, z' '-x, -y, z+1/2' '-x+y, -x, z' 'y, -x+y, z+1/2' '-y, -x, -z+1/2' 'x-y, -y, -z' 'x, x-y, -z+1/2' 'y, x, -z' '-x+y, y, -z+1/2' '-x, -x+y, -z' _cell_length_a 22.275(13) _cell_length_b 22.275(13) _cell_length_c 26.024(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 11183(11) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22059 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 30.2 _exptl_crystal_description needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4512 _exptl_absorpt_coefficient_mu 0.644 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9503 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device 'AFC12 (Right): Kappa 3 circle' _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_reflns_number 76517 _diffrn_reflns_av_R_equivalents 0.0963 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 20.81 _reflns_number_total 3922 _reflns_number_gt 3882 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_cell_refinement ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_data_reduction ; CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The structure was solved by direct methods. It is a polymeric structure composed of [Ag2(C31H24N6O)2] units which are connected together via Ag...Ag interactions. There are also two [PF6]- anions per Ag2 complex. The space group was confirmed by Platon. All hydrogens were added in calculated positions. The structure was inverted to bring the Flack parameter close to 0. The structure grows such that three of the Ag2 complexes are present in the Unit cell. Although some alerts in the cif check suggest close F - F contacts these are not real. The structure contained solvent accessible voids and therefore the Platon Squeeze program was employed: loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.129 9 5 ' ' 2 0.000 0.000 0.371 9 5 ' ' 3 0.000 0.000 0.629 9 5 ' ' 4 0.000 0.000 0.871 9 5 ' ' 5 0.333 0.667 0.750 643 191 ' ' 6 0.333 0.667 0.250 415 165 ' ' 7 0.667 0.333 0.250 643 192 ' ' 8 0.667 0.333 0.750 415 166 ' ' _platon_squeeze_details All 6 and 5 membered rings were fixed using geometric restraints as were the anions. Global displacement restraints have been used to achieve a consistent model. One pyridine ring is completely disordered over two sites (N31-C36 and N31B-C36B) (54:46) The crystals were very small needles and were weakly diffracting. The data was obtained firstly at Sheffield and then at a more powerful machine at the NCS in Southampton. The data was the best achievable and was cut at an appropriate point (1.00 A). 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^)+(0.1026P)^2^+43.5933P] 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 0.09(9) _refine_ls_number_reflns 3922 _refine_ls_number_parameters 394 _refine_ls_number_restraints 589 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0884 _refine_ls_wR_factor_ref 0.2262 _refine_ls_wR_factor_gt 0.2250 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.112 _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 0.95429(5) 0.68518(6) 0.95215(4) 0.0906(4) Uani 1 1 d . . . N11 N 1.0463(4) 0.6807(4) 0.9145(3) 0.0895(12) Uani 1 1 d GU A . C12 C 1.0746(4) 0.7216(4) 0.8710(3) 0.0901(11) Uani 1 1 d GU . . C13 C 1.1259(4) 0.7176(4) 0.8433(3) 0.0913(12) Uani 1 1 d GU A . H13 H 1.1453 0.7456 0.8136 0.110 Uiso 1 1 calc R . . C14 C 1.1488(4) 0.6729(5) 0.8591(3) 0.0917(13) Uani 1 1 d GU . . H14 H 1.1839 0.6702 0.8401 0.110 Uiso 1 1 calc R A . C15 C 1.1205(4) 0.6320(4) 0.9025(3) 0.0911(13) Uani 1 1 d GU A . H15 H 1.1361 0.6014 0.9133 0.109 Uiso 1 1 calc R . . C16 C 1.0692(4) 0.6360(4) 0.9303(3) 0.0902(13) Uani 1 1 d GU . . H16 H 1.0498 0.6081 0.9600 0.108 Uiso 1 1 calc R A . N21 N 0.9791(4) 0.8139(4) 0.8594(3) 0.0897(11) Uani 1 1 d GU . . N22 N 0.9908(4) 0.7613(4) 0.8795(3) 0.0892(11) Uani 1 1 d GU A . C23 C 1.0519(5) 0.7688(5) 0.8565(3) 0.0898(11) Uani 1 1 d GU A . C24 C 1.0781(4) 0.8259(5) 0.8222(3) 0.0908(12) Uani 1 1 d GU A . H24 H 1.1185 0.8426 0.8016 0.109 Uiso 1 1 calc R . . C25 C 1.0331(5) 0.8538(4) 0.8239(3) 0.0907(12) Uani 1 1 d GU A . H25 H 1.0381 0.8924 0.8048 0.109 Uiso 1 1 calc R . . C26 C 0.9211(7) 0.8200(7) 0.8722(5) 0.0899(11) Uani 1 1 d U A . H26A H 0.9293 0.8654 0.8598 0.108 Uiso 1 1 calc R . . H26B H 0.9175 0.8199 0.9101 0.108 Uiso 1 1 calc R . . N31 N 0.8809(6) 0.7105(4) 1.0095(3) 0.0912(12) Uani 0.54(5) 1 d PGU A 1 C32 C 0.8197(5) 0.6530(4) 1.0258(7) 0.0916(12) Uani 0.54(5) 1 d PGU A 1 C33 C 0.7790(7) 0.6605(5) 1.0628(12) 0.0916(13) Uani 0.54(5) 1 d PGU A 1 H33 H 0.7372 0.6213 1.0740 0.110 Uiso 0.54(5) 1 calc PR A 1 C34 C 0.7996(10) 0.7254(6) 1.0837(13) 0.0915(13) Uani 0.54(5) 1 d PGU A 1 H34 H 0.7718 0.7306 1.1090 0.110 Uiso 0.54(5) 1 calc PR A 1 C35 C 0.8608(7) 0.7829(4) 1.0674(9) 0.0913(13) Uani 0.54(5) 1 d PGU A 1 H35 H 0.8749 0.8272 1.0816 0.110 Uiso 0.54(5) 1 calc PR A 1 C36 C 0.9015(4) 0.7754(4) 1.0303(4) 0.0913(13) Uani 0.54(5) 1 d PGU A 1 H36 H 0.9433 0.8146 1.0191 0.110 Uiso 0.54(5) 1 calc PR A 1 N31B N 0.8883(6) 0.7128(5) 1.0089(3) 0.0912(12) Uani 0.46(5) 1 d PGU A 2 C32C C 0.8224(5) 0.6565(4) 1.0171(6) 0.0916(12) Uani 0.46(5) 1 d PGU A 2 C33B C 0.7734(4) 0.6654(5) 1.0440(13) 0.0916(12) Uani 0.46(5) 1 d PGU A 2 H33B H 0.7284 0.6269 1.0497 0.110 Uiso 0.46(5) 1 calc PR A 2 C34B C 0.7904(6) 0.7305(6) 1.0626(15) 0.0915(13) Uani 0.46(5) 1 d PGU A 2 H34B H 0.7569 0.7365 1.0810 0.110 Uiso 0.46(5) 1 calc PR A 2 C35B C 0.8563(5) 0.7867(4) 1.0544(10) 0.0914(13) Uani 0.46(5) 1 d PGU A 2 H35B H 0.8679 0.8312 1.0671 0.110 Uiso 0.46(5) 1 calc PR A 2 C36B C 0.9052(5) 0.7779(4) 1.0275(4) 0.0913(13) Uani 0.46(5) 1 d PGU A 2 H36B H 0.9503 0.8163 1.0218 0.110 Uiso 0.46(5) 1 calc PR A 2 N41 N 0.8199(4) 0.5123(4) 0.9533(3) 0.0947(12) Uani 1 1 d GU . . N42 N 0.8526(3) 0.5818(4) 0.9713(3) 0.0932(12) Uani 1 1 d GU A . C43 C 0.8030(5) 0.5904(4) 0.9997(3) 0.0929(11) Uani 1 1 d GU A . C44 C 0.7397(4) 0.5263(5) 0.9994(4) 0.0948(13) Uani 1 1 d GU A . H44 H 0.6977 0.5172 1.0155 0.114 Uiso 1 1 calc R . . C45 C 0.7501(4) 0.4780(3) 0.9708(4) 0.0954(13) Uani 1 1 d GU A . H45 H 0.7164 0.4310 0.9643 0.115 Uiso 1 1 calc R . . C46 C 0.8594(8) 0.4903(8) 0.9243(6) 0.0955(12) Uani 1 1 d U A . H46A H 0.8311 0.4396 0.9189 0.115 Uiso 1 1 calc R . . H46B H 0.9006 0.4991 0.9447 0.115 Uiso 1 1 calc R . . C51 C 0.8496(3) 0.7619(3) 0.8501(3) 0.0902(12) Uani 1 1 d GU . . C52 C 0.8322(4) 0.7715(3) 0.8007(3) 0.0909(14) Uani 1 1 d GU A . H52 H 0.8615 0.8132 0.7826 0.109 Uiso 1 1 calc R . . C53 C 0.7718(4) 0.7203(4) 0.7778(2) 0.0916(14) Uani 1 1 d GU A . H53 H 0.7598 0.7269 0.7441 0.110 Uiso 1 1 calc R . . C54 C 0.7289(3) 0.6593(3) 0.8042(3) 0.0917(14) Uani 1 1 d GU A . C55 C 0.7464(3) 0.6497(3) 0.8536(2) 0.0912(14) Uani 1 1 d GU A . H55 H 0.7171 0.6080 0.8717 0.109 Uiso 1 1 calc R . . C56 C 0.8067(3) 0.7009(3) 0.87652(19) 0.0905(14) Uani 1 1 d GU A . H56 H 0.8187 0.6943 0.9103 0.109 Uiso 1 1 calc R . . C61 C 0.8839(4) 0.5251(3) 0.8720(3) 0.0940(13) Uani 1 1 d GU A . C62 C 0.8549(3) 0.5608(2) 0.8488(2) 0.0938(13) Uani 1 1 d GU A . H62 H 0.8209 0.5668 0.8666 0.113 Uiso 1 1 calc R . . C63 C 0.8754(3) 0.5878(3) 0.79965(19) 0.0935(14) Uani 1 1 d GU A . H63 H 0.8555 0.6122 0.7838 0.112 Uiso 1 1 calc R . . C64 C 0.9250(3) 0.5791(3) 0.7736(2) 0.0935(14) Uani 1 1 d GU . . C65 C 0.9541(3) 0.5434(3) 0.7968(3) 0.0934(14) Uani 1 1 d GU A . H65 H 0.9880 0.5374 0.7790 0.112 Uiso 1 1 calc R . . C66 C 0.9336(4) 0.5164(3) 0.8460(3) 0.0939(13) Uani 1 1 d GU A . H66 H 0.9535 0.4919 0.8618 0.113 Uiso 1 1 calc R . . C71 C 0.6572(6) 0.6027(7) 0.7809(5) 0.0932(16) Uani 1 1 d DU . . O72 O 0.6067(5) 0.5738(5) 0.8102(3) 0.101(2) Uani 1 1 d DU A . P11 P 0.4296(2) 0.0000 1.0000 0.1057(17) Uani 1 2 d SDU . . F12 F 0.3593(4) 0.0000 1.0000 0.214(7) Uani 1 2 d SDU . . F13 F 0.3980(5) -0.0611(5) 0.9588(4) 0.156(4) Uani 1 1 d DU . . F14 F 0.5007(4) 0.0000 1.0000 0.150(5) Uani 1 2 d SDU . . F15 F 0.4554(8) 0.0551(6) 0.9554(4) 0.207(5) Uani 1 1 d DU . . P21 P 0.3333 0.6667 0.9070(5) 0.095(4) Uani 0.50 3 d SPDU . . F22 F 0.2957(10) 0.6007(8) 0.8721(7) 0.154(7) Uani 0.50 1 d PDU . . F23 F 0.3656(8) 0.6329(8) 0.9414(6) 0.132(6) Uani 0.50 1 d PDU . . P31 P 1.0000 1.0000 0.0000 0.094(3) Uani 1 6 d SDU . . F32 F 0.9672(6) 0.9324(4) -0.0350(3) 0.153(4) Uani 1 1 d DU . . P41 P 1.0000 1.0000 0.7500 0.098(3) Uani 1 6 d SDU . . F42 F 0.9397(5) 0.9372(5) 0.7818(4) 0.168(4) Uani 1 1 d DU . . 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 0.0898(7) 0.1064(8) 0.0856(7) 0.0000(6) 0.0013(6) 0.0567(6) N11 0.090(3) 0.099(3) 0.085(2) -0.006(2) -0.007(2) 0.051(2) C12 0.090(2) 0.099(3) 0.085(2) -0.006(2) -0.006(2) 0.050(2) C13 0.091(3) 0.100(3) 0.086(3) -0.006(2) -0.006(2) 0.050(2) C14 0.091(3) 0.101(3) 0.087(3) -0.006(2) -0.005(2) 0.051(2) C15 0.090(3) 0.100(3) 0.087(3) -0.006(2) -0.006(2) 0.051(2) C16 0.090(3) 0.099(3) 0.086(3) -0.006(2) -0.007(2) 0.051(2) N21 0.090(2) 0.099(2) 0.083(2) -0.0029(19) -0.0075(18) 0.0501(19) N22 0.090(2) 0.099(3) 0.083(2) -0.004(2) -0.0073(19) 0.050(2) C23 0.090(2) 0.100(2) 0.083(2) -0.0045(19) -0.0067(19) 0.050(2) C24 0.091(2) 0.100(3) 0.083(2) -0.004(2) -0.007(2) 0.049(2) C25 0.091(2) 0.100(3) 0.083(2) -0.003(2) -0.007(2) 0.049(2) C26 0.090(2) 0.100(3) 0.083(2) -0.002(2) -0.0072(19) 0.050(2) N31 0.091(2) 0.084(2) 0.106(3) -0.001(2) -0.010(2) 0.050(2) C32 0.092(2) 0.084(2) 0.106(3) -0.001(2) -0.010(2) 0.0494(19) C33 0.091(2) 0.085(2) 0.106(3) -0.001(2) -0.010(2) 0.049(2) C34 0.091(2) 0.085(2) 0.106(3) -0.001(2) -0.010(2) 0.049(2) C35 0.091(2) 0.084(2) 0.106(3) -0.001(2) -0.010(2) 0.050(2) C36 0.091(2) 0.084(2) 0.106(3) -0.001(2) -0.010(2) 0.049(2) N31B 0.091(2) 0.084(2) 0.106(3) -0.001(2) -0.010(2) 0.050(2) C32C 0.092(2) 0.085(2) 0.106(3) -0.001(2) -0.010(2) 0.0493(19) C33B 0.091(2) 0.085(2) 0.106(3) -0.001(2) -0.010(2) 0.049(2) C34B 0.091(2) 0.085(2) 0.106(3) -0.001(2) -0.010(2) 0.049(2) C35B 0.091(2) 0.085(2) 0.106(3) -0.001(2) -0.010(2) 0.049(2) C36B 0.091(2) 0.084(2) 0.106(3) -0.001(2) -0.010(2) 0.049(2) N41 0.095(2) 0.085(2) 0.108(3) -0.003(2) -0.010(2) 0.0492(19) N42 0.094(2) 0.085(2) 0.107(3) -0.002(2) -0.010(2) 0.049(2) C43 0.093(2) 0.085(2) 0.107(3) -0.002(2) -0.010(2) 0.0487(19) C44 0.094(2) 0.086(2) 0.108(3) -0.002(2) -0.009(2) 0.048(2) C45 0.095(2) 0.086(2) 0.108(3) -0.003(2) -0.009(2) 0.048(2) C46 0.097(2) 0.086(2) 0.109(3) -0.005(2) -0.010(2) 0.050(2) C51 0.090(2) 0.100(3) 0.084(2) -0.002(2) -0.0062(19) 0.050(2) C52 0.090(3) 0.101(3) 0.084(2) -0.002(2) -0.006(2) 0.049(2) C53 0.090(3) 0.101(3) 0.084(3) -0.001(2) -0.006(2) 0.048(2) C54 0.090(3) 0.102(3) 0.085(2) -0.001(2) -0.005(2) 0.049(2) C55 0.090(3) 0.101(3) 0.085(3) -0.001(2) -0.005(2) 0.050(2) C56 0.090(3) 0.100(3) 0.084(2) -0.002(2) -0.005(2) 0.050(2) C61 0.097(3) 0.086(2) 0.109(3) -0.006(2) -0.010(2) 0.053(2) C62 0.097(3) 0.086(3) 0.109(3) -0.007(2) -0.010(2) 0.054(2) C63 0.097(3) 0.086(3) 0.109(3) -0.007(2) -0.010(3) 0.054(2) C64 0.097(3) 0.086(3) 0.109(3) -0.007(2) -0.010(2) 0.054(2) C65 0.097(3) 0.086(3) 0.109(3) -0.007(2) -0.010(2) 0.054(2) C66 0.097(3) 0.086(3) 0.109(3) -0.006(2) -0.011(2) 0.054(2) C71 0.090(3) 0.103(3) 0.085(3) -0.001(2) -0.003(2) 0.047(2) O72 0.094(3) 0.110(4) 0.088(3) 0.000(3) 0.001(3) 0.042(3) P11 0.079(2) 0.130(5) 0.124(4) -0.008(4) -0.0042(19) 0.065(2) F12 0.123(6) 0.250(16) 0.310(18) -0.117(14) -0.058(7) 0.125(8) F13 0.108(6) 0.171(8) 0.178(9) -0.044(8) 0.010(6) 0.061(6) F14 0.114(5) 0.160(11) 0.192(12) -0.004(10) -0.002(5) 0.080(6) F15 0.256(13) 0.181(10) 0.157(9) 0.025(8) -0.040(9) 0.090(10) P21 0.070(4) 0.070(4) 0.146(11) 0.000 0.000 0.035(2) F22 0.152(15) 0.093(11) 0.176(15) -0.027(10) 0.012(12) 0.031(11) F23 0.078(10) 0.118(12) 0.204(16) 0.013(12) -0.008(10) 0.052(9) P31 0.083(4) 0.083(4) 0.116(7) 0.000 0.000 0.0417(18) F32 0.196(10) 0.085(5) 0.158(8) -0.031(5) -0.055(7) 0.055(6) P41 0.058(3) 0.058(3) 0.178(10) 0.000 0.000 0.0290(15) F42 0.121(8) 0.114(7) 0.254(12) 0.073(7) 0.004(7) 0.047(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 N11 2.318(6) . ? Ag1 N42 2.338(7) . ? Ag1 N31B 2.371(9) . ? Ag1 N22 2.395(6) . ? Ag1 N31 2.476(9) . ? Ag1 Ag1 3.052(3) 12_767 ? N11 C12 1.3900 . ? N11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 C23 1.427(9) . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C15 1.3900 . ? C14 H14 0.9500 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C26 1.404(15) . ? N21 N22 1.4200 . ? N21 C25 1.4200 . ? N22 C23 1.4200 . ? C23 C24 1.4200 . ? C24 C25 1.4200 . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C51 1.575(15) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N31 C32 1.3900 . ? N31 C36 1.3900 . ? C32 C33 1.3900 . ? C32 C43 1.422(9) . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? N31B C32C 1.3901 . ? N31B C36B 1.3901 . ? C32C C43 1.387(9) . ? C32C C33B 1.3899 . ? C33B C34B 1.3901 . ? C33B H33B 0.9500 . ? C34B C35B 1.3900 . ? C34B H34B 0.9500 . ? C35B C36B 1.3900 . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? N41 C45 1.4200 . ? N41 N42 1.4200 . ? N41 C46 1.422(15) . ? N42 C43 1.4200 . ? C43 C44 1.4200 . ? C44 C45 1.4200 . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C61 1.526(16) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 C71 1.580(15) . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C62 1.3899 . ? C61 C66 1.3901 . ? C62 C63 1.3900 . ? C62 H62 0.9500 . ? C63 C64 1.3900 . ? C63 H63 0.9500 . ? C64 C65 1.3900 . ? C64 C71 1.504(14) 11_656 ? C65 C66 1.3900 . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 O72 1.239(8) . ? C71 C64 1.505(18) 11_656 ? P11 F12 1.565(9) . ? P11 F15 1.574(8) . ? P11 F15 1.574(8) 8_557 ? P11 F14 1.585(9) . ? P11 F13 1.594(7) 8_557 ? P11 F13 1.594(7) . ? P21 F23 1.558(9) 3_665 ? P21 F23 1.558(9) 5_565 ? P21 F23 1.558(9) . ? P21 F22 1.566(9) 5_565 ? P21 F22 1.566(9) . ? P21 F22 1.566(9) 3_665 ? P31 F32 1.590(6) . ? P31 F32 1.590(6) 10 ? P31 F32 1.590(6) 8_675 ? P31 F32 1.590(6) 3_765 ? P31 F32 1.590(6) 5_675 ? P31 F32 1.590(6) 12_765 ? P41 F42 1.602(7) 11_656 ? P41 F42 1.602(7) 3_765 ? P41 F42 1.602(7) 9_566 ? P41 F42 1.602(7) 5_675 ? P41 F42 1.602(7) 7_776 ? P41 F42 1.602(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ag1 N42 119.4(3) . . ? N11 Ag1 N31B 161.9(4) . . ? N42 Ag1 N31B 72.6(3) . . ? N11 Ag1 N22 72.7(3) . . ? N42 Ag1 N22 133.2(3) . . ? N31B Ag1 N22 110.0(3) . . ? N11 Ag1 N31 164.2(3) . . ? N42 Ag1 N31 70.8(3) . . ? N31B Ag1 N31 2.4 . . ? N22 Ag1 N31 110.1(3) . . ? N11 Ag1 Ag1 84.4(2) . 12_767 ? N42 Ag1 Ag1 108.1(2) . 12_767 ? N31B Ag1 Ag1 78.6(3) . 12_767 ? N22 Ag1 Ag1 118.3(2) . 12_767 ? N31 Ag1 Ag1 80.7(2) . 12_767 ? C12 N11 C16 120.0 . . ? C12 N11 Ag1 116.0(4) . . ? C16 N11 Ag1 123.8(4) . . ? C13 C12 N11 120.0 . . ? C13 C12 C23 120.9(7) . . ? N11 C12 C23 119.1(6) . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 N11 120.0 . . ? C15 C16 H16 120.0 . . ? N11 C16 H16 120.0 . . ? C26 N21 N22 123.2(8) . . ? C26 N21 C25 128.7(8) . . ? N22 N21 C25 108.0 . . ? N21 N22 C23 108.0 . . ? N21 N22 Ag1 137.6(5) . . ? C23 N22 Ag1 112.4(5) . . ? C24 C23 N22 108.0 . . ? C24 C23 C12 133.6(7) . . ? N22 C23 C12 118.4(7) . . ? C25 C24 C23 108.0 . . ? C25 C24 H24 126.0 . . ? C23 C24 H24 126.0 . . ? C24 C25 N21 108.0 . . ? C24 C25 H25 126.0 . . ? N21 C25 H25 126.0 . . ? N21 C26 C51 115.8(10) . . ? N21 C26 H26A 108.3 . . ? C51 C26 H26A 108.3 . . ? N21 C26 H26B 108.3 . . ? C51 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C32 N31 C36 120.0 . . ? C32 N31 Ag1 115.5(4) . . ? C36 N31 Ag1 124.0(5) . . ? N31 C32 C33 120.0 . . ? N31 C32 C43 114.3(8) . . ? C33 C32 C43 125.6(9) . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 N31 120.0 . . ? C35 C36 H36 120.0 . . ? N31 C36 H36 120.0 . . ? C32C N31B C36B 120.0 . . ? C32C N31B Ag1 112.0(5) . . ? C36B N31B Ag1 127.4(5) . . ? C43 C32C C33B 117.8(9) . . ? C43 C32C N31B 122.2(8) . . ? C33B C32C N31B 120.0 . . ? C32C C33B C34B 120.0 . . ? C32C C33B H33B 120.0 . . ? C34B C33B H33B 120.0 . . ? C35B C34B C33B 120.0 . . ? C35B C34B H34B 120.0 . . ? C33B C34B H34B 120.0 . . ? C36B C35B C34B 120.0 . . ? C36B C35B H35B 120.0 . . ? C34B C35B H35B 120.0 . . ? C35B C36B N31B 120.0 . . ? C35B C36B H36B 120.0 . . ? N31B C36B H36B 120.0 . . ? C45 N41 N42 108.0 . . ? C45 N41 C46 133.1(8) . . ? N42 N41 C46 118.8(8) . . ? C43 N42 N41 108.0 . . ? C43 N42 Ag1 114.4(4) . . ? N41 N42 Ag1 136.1(5) . . ? C32C C43 N42 117.7(8) . . ? C32C C43 C44 134.0(8) . . ? N42 C43 C44 108.0 . . ? C32C C43 C32 9.50(7) . . ? N42 C43 C32 122.8(7) . . ? C44 C43 C32 129.1(7) . . ? C43 C44 C45 108.0 . . ? C43 C44 H44 126.0 . . ? C45 C44 H44 126.0 . . ? N41 C45 C44 108.0 . . ? N41 C45 H45 126.0 . . ? C44 C45 H45 126.0 . . ? N41 C46 C61 115.2(10) . . ? N41 C46 H46A 108.5 . . ? C61 C46 H46A 108.5 . . ? N41 C46 H46B 108.5 . . ? C61 C46 H46B 108.5 . . ? H46A C46 H46B 107.5 . . ? C52 C51 C56 120.0 . . ? C52 C51 C26 117.2(7) . . ? C56 C51 C26 122.7(7) . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 C71 118.8(6) . . ? C53 C54 C71 121.1(6) . . ? C54 C55 C56 120.0 . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 C46 121.8(6) . . ? C66 C61 C46 118.1(6) . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 C71 122.3(5) . 11_656 ? C65 C64 C71 117.5(5) . 11_656 ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? O72 C71 C64 121.9(11) . 11_656 ? O72 C71 C54 118.1(11) . . ? C64 C71 C54 119.5(8) 11_656 . ? F12 P11 F15 88.6(6) . . ? F12 P11 F15 88.6(6) . 8_557 ? F15 P11 F15 177.2(13) . 8_557 ? F12 P11 F14 180.000(5) . . ? F15 P11 F14 91.4(6) . . ? F15 P11 F14 91.4(6) 8_557 . ? F12 P11 F13 89.2(4) . 8_557 ? F15 P11 F13 89.8(6) . 8_557 ? F15 P11 F13 90.2(6) 8_557 8_557 ? F14 P11 F13 90.8(4) . 8_557 ? F12 P11 F13 89.2(4) . . ? F15 P11 F13 90.2(6) . . ? F15 P11 F13 89.8(7) 8_557 . ? F14 P11 F13 90.8(4) . . ? F13 P11 F13 178.4(8) 8_557 . ? F23 P21 F23 90.2(11) 3_665 5_565 ? F23 P21 F23 90.2(11) 3_665 . ? F23 P21 F23 90.2(11) 5_565 . ? F23 P21 F22 87.8(10) 3_665 5_565 ? F23 P21 F22 92.3(6) 5_565 5_565 ? F23 P21 F22 176.8(9) . 5_565 ? F23 P21 F22 176.8(9) 3_665 . ? F23 P21 F22 87.8(11) 5_565 . ? F23 P21 F22 92.3(6) . . ? F22 P21 F22 89.8(12) 5_565 . ? F23 P21 F22 92.3(6) 3_665 3_665 ? F23 P21 F22 176.8(9) 5_565 3_665 ? F23 P21 F22 87.8(10) . 3_665 ? F22 P21 F22 89.8(12) 5_565 3_665 ? F22 P21 F22 89.8(12) . 3_665 ? F32 P31 F32 90.7(9) . 10 ? F32 P31 F32 178.4(9) . 8_675 ? F32 P31 F32 90.5(5) 10 8_675 ? F32 P31 F32 90.5(5) . 3_765 ? F32 P31 F32 178.4(9) 10 3_765 ? F32 P31 F32 88.4(8) 8_675 3_765 ? F32 P31 F32 90.5(5) . 5_675 ? F32 P31 F32 88.4(8) 10 5_675 ? F32 P31 F32 90.7(9) 8_675 5_675 ? F32 P31 F32 90.5(5) 3_765 5_675 ? F32 P31 F32 88.4(7) . 12_765 ? F32 P31 F32 90.5(5) 10 12_765 ? F32 P31 F32 90.5(5) 8_675 12_765 ? F32 P31 F32 90.7(9) 3_765 12_765 ? F32 P31 F32 178.4(9) 5_675 12_765 ? F42 P41 F42 86.8(8) 11_656 3_765 ? F42 P41 F42 95.7(6) 11_656 9_566 ? F42 P41 F42 176.6(8) 3_765 9_566 ? F42 P41 F42 176.6(8) 11_656 5_675 ? F42 P41 F42 95.7(6) 3_765 5_675 ? F42 P41 F42 81.8(9) 9_566 5_675 ? F42 P41 F42 95.7(6) 11_656 7_776 ? F42 P41 F42 81.8(9) 3_765 7_776 ? F42 P41 F42 95.7(6) 9_566 7_776 ? F42 P41 F42 86.8(8) 5_675 7_776 ? F42 P41 F42 81.8(9) 11_656 . ? F42 P41 F42 95.7(6) 3_765 . ? F42 P41 F42 86.8(8) 9_566 . ? F42 P41 F42 95.7(6) 5_675 . ? F42 P41 F42 176.6(8) 7_776 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N42 Ag1 N11 C12 129.9(5) . . . . ? N31B Ag1 N11 C12 -102.1(10) . . . . ? N22 Ag1 N11 C12 -0.4(4) . . . . ? N31 Ag1 N11 C12 -103.1(10) . . . . ? Ag1 Ag1 N11 C12 -122.4(4) 12_767 . . . ? N42 Ag1 N11 C16 -44.3(6) . . . . ? N31B Ag1 N11 C16 83.8(11) . . . . ? N22 Ag1 N11 C16 -174.6(5) . . . . ? N31 Ag1 N11 C16 82.8(12) . . . . ? Ag1 Ag1 N11 C16 63.4(4) 12_767 . . . ? C16 N11 C12 C13 0.0 . . . . ? Ag1 N11 C12 C13 -174.4(5) . . . . ? C16 N11 C12 C23 -178.0(9) . . . . ? Ag1 N11 C12 C23 7.6(8) . . . . ? N11 C12 C13 C14 0.0 . . . . ? C23 C12 C13 C14 178.0(9) . . . . ? C12 C13 C14 C15 0.0 . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C15 C16 N11 0.0 . . . . ? C12 N11 C16 C15 0.0 . . . . ? Ag1 N11 C16 C15 173.9(6) . . . . ? C26 N21 N22 C23 177.1(11) . . . . ? C25 N21 N22 C23 0.0 . . . . ? C26 N21 N22 Ag1 -21.2(12) . . . . ? C25 N21 N22 Ag1 161.7(8) . . . . ? N11 Ag1 N22 N21 -167.6(8) . . . . ? N42 Ag1 N22 N21 78.1(8) . . . . ? N31B Ag1 N22 N21 -6.5(8) . . . . ? N31 Ag1 N22 N21 -4.0(8) . . . . ? Ag1 Ag1 N22 N21 -94.1(7) 12_767 . . . ? N11 Ag1 N22 C23 -6.4(5) . . . . ? N42 Ag1 N22 C23 -120.7(5) . . . . ? N31B Ag1 N22 C23 154.6(5) . . . . ? N31 Ag1 N22 C23 157.2(5) . . . . ? Ag1 Ag1 N22 C23 67.1(5) 12_767 . . . ? N21 N22 C23 C24 0.0 . . . . ? Ag1 N22 C23 C24 -166.7(6) . . . . ? N21 N22 C23 C12 179.6(9) . . . . ? Ag1 N22 C23 C12 12.9(8) . . . . ? C13 C12 C23 C24 -12.7(12) . . . . ? N11 C12 C23 C24 165.3(7) . . . . ? C13 C12 C23 N22 167.8(5) . . . . ? N11 C12 C23 N22 -14.2(10) . . . . ? N22 C23 C24 C25 0.0 . . . . ? C12 C23 C24 C25 -179.5(11) . . . . ? C23 C24 C25 N21 0.0 . . . . ? C26 N21 C25 C24 -176.9(11) . . . . ? N22 N21 C25 C24 0.0 . . . . ? N22 N21 C26 C51 -70.2(13) . . . . ? C25 N21 C26 C51 106.3(11) . . . . ? N11 Ag1 N31 C32 -130.0(14) . . . . ? N42 Ag1 N31 C32 2.6(9) . . . . ? N31B Ag1 N31 C32 -137.7(5) . . . . ? N22 Ag1 N31 C32 132.7(8) . . . . ? Ag1 Ag1 N31 C32 -110.5(9) 12_767 . . . ? N11 Ag1 N31 C36 41.8(13) . . . . ? N42 Ag1 N31 C36 174.3(7) . . . . ? N31B Ag1 N31 C36 34.0(16) . . . . ? N22 Ag1 N31 C36 -55.6(7) . . . . ? Ag1 Ag1 N31 C36 61.3(6) 12_767 . . . ? C36 N31 C32 C33 0.0 . . . . ? Ag1 N31 C32 C33 172.1(12) . . . . ? C36 N31 C32 C43 177.2(9) . . . . ? Ag1 N31 C32 C43 -10.7(14) . . . . ? N31 C32 C33 C34 0.0 . . . . ? C43 C32 C33 C34 -176.8(10) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 N31 0.0 . . . . ? C32 N31 C36 C35 0.0 . . . . ? Ag1 N31 C36 C35 -171.4(13) . . . . ? N11 Ag1 N31B C32C -142.3(11) . . . . ? N42 Ag1 N31B C32C -8.3(8) . . . . ? N22 Ag1 N31B C32C 122.2(8) . . . . ? N31 Ag1 N31B C32C 30.9(5) . . . . ? Ag1 Ag1 N31B C32C -121.6(8) 12_767 . . . ? N11 Ag1 N31B C36B 46.6(13) . . . . ? N42 Ag1 N31B C36B -179.4(8) . . . . ? N22 Ag1 N31B C36B -48.9(8) . . . . ? N31 Ag1 N31B C36B -140.2(17) . . . . ? Ag1 Ag1 N31B C36B 67.3(7) 12_767 . . . ? C36B N31B C32C C43 -179.5(10) . . . . ? Ag1 N31B C32C C43 8.7(16) . . . . ? C36B N31B C32C C33B 0.0 . . . . ? Ag1 N31B C32C C33B -171.8(12) . . . . ? C43 C32C C33B C34B 179.5(10) . . . . ? N31B C32C C33B C34B 0.0 . . . . ? C32C C33B C34B C35B 0.0 . . . . ? C33B C34B C35B C36B 0.0 . . . . ? C34B C35B C36B N31B 0.0 . . . . ? C32C N31B C36B C35B 0.0 . . . . ? Ag1 N31B C36B C35B 170.4(14) . . . . ? C45 N41 N42 C43 0.0 . . . . ? C46 N41 N42 C43 -179.0(10) . . . . ? C45 N41 N42 Ag1 -164.7(8) . . . . ? C46 N41 N42 Ag1 16.4(11) . . . . ? N11 Ag1 N42 C43 172.8(4) . . . . ? N31B Ag1 N42 C43 7.6(5) . . . . ? N22 Ag1 N42 C43 -93.8(6) . . . . ? N31 Ag1 N42 C43 6.0(5) . . . . ? Ag1 Ag1 N42 C43 79.0(5) 12_767 . . . ? N11 Ag1 N42 N41 -23.3(8) . . . . ? N31B Ag1 N42 N41 171.6(8) . . . . ? N22 Ag1 N42 N41 70.1(8) . . . . ? N31 Ag1 N42 N41 170.0(8) . . . . ? Ag1 Ag1 N42 N41 -117.1(7) 12_767 . . . ? C33B C32C C43 N42 178.6(12) . . . . ? N31B C32C C43 N42 -1.9(17) . . . . ? C33B C32C C43 C44 5.8(13) . . . . ? N31B C32C C43 C44 -174.7(9) . . . . ? C33B C32C C43 C32 -56.5(5) . . . . ? N31B C32C C43 C32 123.0(6) . . . . ? N41 N42 C43 C32C -174.6(11) . . . . ? Ag1 N42 C43 C32C -6.2(10) . . . . ? N41 N42 C43 C44 0.0 . . . . ? Ag1 N42 C43 C44 168.4(6) . . . . ? N41 N42 C43 C32 176.2(12) . . . . ? Ag1 N42 C43 C32 -15.4(11) . . . . ? N31 C32 C43 C32C -41.9(5) . . . . ? C33 C32 C43 C32C 135.1(5) . . . . ? N31 C32 C43 N42 17.8(16) . . . . ? C33 C32 C43 N42 -165.2(13) . . . . ? N31 C32 C43 C44 -166.8(8) . . . . ? C33 C32 C43 C44 10.1(13) . . . . ? C32C C43 C44 C45 173.3(14) . . . . ? N42 C43 C44 C45 0.0 . . . . ? C32 C43 C44 C45 -175.9(13) . . . . ? N42 N41 C45 C44 0.0 . . . . ? C46 N41 C45 C44 178.8(12) . . . . ? C43 C44 C45 N41 0.0 . . . . ? C45 N41 C46 C61 115.5(11) . . . . ? N42 N41 C46 C61 -65.8(13) . . . . ? N21 C26 C51 C52 -85.7(11) . . . . ? N21 C26 C51 C56 90.3(11) . . . . ? C56 C51 C52 C53 0.0 . . . . ? C26 C51 C52 C53 176.1(6) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C52 C53 C54 C71 175.2(7) . . . . ? C53 C54 C55 C56 0.0 . . . . ? C71 C54 C55 C56 -175.3(6) . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? C26 C51 C56 C55 -175.9(7) . . . . ? N41 C46 C61 C62 -16.5(14) . . . . ? N41 C46 C61 C66 167.7(8) . . . . ? C66 C61 C62 C63 0.0 . . . . ? C46 C61 C62 C63 -175.7(8) . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C62 C63 C64 C71 175.6(8) . . . 11_656 ? C63 C64 C65 C66 0.0 . . . . ? C71 C64 C65 C66 -175.8(8) 11_656 . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? C46 C61 C66 C65 175.9(8) . . . . ? C55 C54 C71 O72 36.2(15) . . . . ? C53 C54 C71 O72 -139.1(10) . . . . ? C55 C54 C71 C64 -135.9(9) . . . 11_656 ? C53 C54 C71 C64 48.8(13) . . . 11_656 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.531 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.084 #===END