# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Mike Ward' 'Harry Adams' 'Stephen P. Argent' 'Lindsay P. Harding' 'J. Jeffery' 'T. Riis-Johannessen' _publ_contact_author_name 'Prof Mike Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Dainton Building Sheffield S3 7HF UK ; _publ_contact_author_email M.D.WARD@SHEFFIELD.AC.UK _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Homo- and heteropolynuclear helicates with a '2+3+2'-dentate compartmental ligand ; data_Cu121 _database_code_depnum_ccdc_archive 'CCDC 265432' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H70 Cu3 N22, 4(F6 P), 4(C2 H3 N)' _chemical_formula_sum 'C94 H82 Cu3 F24 N26 P4' _chemical_formula_weight 2346.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.388(4) _cell_length_b 14.590(2) _cell_length_c 22.348(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.943(3) _cell_angle_gamma 90.00 _cell_volume 9788(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7656 _cell_measurement_theta_min 4.658 _cell_measurement_theta_max 50.731 _exptl_crystal_description block _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4764 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7043 _exptl_absorpt_correction_T_max 0.8467 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 53898 _diffrn_reflns_av_R_equivalents 0.0916 _diffrn_reflns_av_sigmaI/netI 0.0968 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.61 _reflns_number_total 11161 _reflns_number_gt 6011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0896P)^2^+29.3028P] 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 11161 _refine_ls_number_parameters 684 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.2156 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.055 _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 Cu1 Cu 0.26482(2) 0.36010(5) 0.34287(3) 0.0493(2) Uani 1 1 d . . . Cu2 Cu 0.0000 0.16940(5) 0.2500 0.0278(2) Uani 1 2 d S . . N111 N 0.23838(14) 0.4477(3) 0.39678(18) 0.0408(10) Uani 1 1 d . . . C112 C 0.21292(16) 0.4096(3) 0.4349(2) 0.0344(11) Uani 1 1 d . . . C113 C 0.18948(17) 0.4623(4) 0.4703(2) 0.0406(12) Uani 1 1 d . . . H113 H 0.1718 0.4338 0.4966 0.049 Uiso 1 1 calc R . . C114 C 0.1917(2) 0.5552(4) 0.4675(3) 0.0550(15) Uani 1 1 d . . . H114 H 0.1762 0.5920 0.4924 0.066 Uiso 1 1 calc R . . C115 C 0.2166(2) 0.5954(4) 0.4286(3) 0.0582(16) Uani 1 1 d . . . H115 H 0.2178 0.6602 0.4251 0.070 Uiso 1 1 calc R . . C116 C 0.2400(2) 0.5392(4) 0.3942(3) 0.0550(16) Uani 1 1 d . . . H116 H 0.2578 0.5669 0.3679 0.066 Uiso 1 1 calc R . . N121 N 0.23305(13) 0.2646(3) 0.39498(16) 0.0328(9) Uani 1 1 d . . . N122 N 0.22839(14) 0.1751(3) 0.40748(17) 0.0364(9) Uani 1 1 d . . . C123 C 0.20419(18) 0.1632(4) 0.4525(2) 0.0404(12) Uani 1 1 d . . . H123 H 0.1963 0.1061 0.4683 0.048 Uiso 1 1 calc R . . C124 C 0.19309(16) 0.2473(4) 0.4713(2) 0.0369(12) Uani 1 1 d . . . H124 H 0.1761 0.2610 0.5025 0.044 Uiso 1 1 calc R . . C125 C 0.21192(15) 0.3099(3) 0.4350(2) 0.0322(11) Uani 1 1 d . . . C131 C 0.21002(16) 0.0886(3) 0.3133(2) 0.0324(11) Uani 1 1 d . . . C132 C 0.17262(18) 0.0358(3) 0.3159(2) 0.0401(12) Uani 1 1 d . . . H132 H 0.1701 0.0029 0.3519 0.048 Uiso 1 1 calc R . . C133 C 0.13845(17) 0.0299(3) 0.2665(2) 0.0382(12) Uani 1 1 d . . . H133 H 0.1131 -0.0072 0.2689 0.046 Uiso 1 1 calc R . . C134 C 0.14158(16) 0.0781(3) 0.2143(2) 0.0330(11) Uani 1 1 d . . . C135 C 0.18004(17) 0.1270(3) 0.2099(2) 0.0368(11) Uani 1 1 d . . . H135 H 0.1833 0.1569 0.1731 0.044 Uiso 1 1 calc R . . C136 C 0.21359(17) 0.1325(3) 0.2589(2) 0.0359(11) Uani 1 1 d . . . H136 H 0.2397 0.1668 0.2555 0.043 Uiso 1 1 calc R . . C137 C 0.24414(18) 0.1049(4) 0.3694(2) 0.0425(12) Uani 1 1 d . . . H13A H 0.2495 0.0471 0.3926 0.051 Uiso 1 1 calc R . . H13B H 0.2727 0.1247 0.3573 0.051 Uiso 1 1 calc R . . C138 C 0.10271(17) 0.0808(3) 0.1625(2) 0.0387(12) Uani 1 1 d . . . H13C H 0.1131 0.0620 0.1244 0.046 Uiso 1 1 calc R . . H13D H 0.0795 0.0368 0.1707 0.046 Uiso 1 1 calc R . . N141 N 0.05679(12) 0.2050(3) 0.19350(16) 0.0299(9) Uani 1 1 d . . . N142 N 0.08354(13) 0.1732(3) 0.15529(16) 0.0329(9) Uani 1 1 d . . . C143 C 0.09517(18) 0.2399(4) 0.1195(2) 0.0432(13) Uani 1 1 d . . . H143 H 0.1142 0.2332 0.0898 0.052 Uiso 1 1 calc R . . C144 C 0.07481(17) 0.3194(4) 0.1332(2) 0.0365(11) Uani 1 1 d . . . H144 H 0.0762 0.3781 0.1151 0.044 Uiso 1 1 calc R . . C145 C 0.05162(15) 0.2941(3) 0.17979(19) 0.0286(10) Uani 1 1 d . . . N151 N 0.0000 0.3032(4) 0.2500 0.0280(12) Uani 1 2 d S . . C152 C 0.02482(15) 0.3503(3) 0.21449(19) 0.0282(10) Uani 1 1 d . . . C153 C 0.02430(16) 0.4456(3) 0.2125(2) 0.0337(11) Uani 1 1 d . . . H153 H 0.0403 0.4779 0.1859 0.040 Uiso 1 1 calc R . . C154 C 0.0000 0.4920(5) 0.2500 0.0358(16) Uani 1 2 d S . . H154 H 0.0000 0.5571 0.2500 0.043 Uiso 1 2 calc SR . . N211 N 0.31552(15) 0.3229(3) 0.3018(2) 0.0464(11) Uani 1 1 d . . . C212 C 0.30616(18) 0.3165(3) 0.2401(2) 0.0401(12) Uani 1 1 d . . . C213 C 0.3371(2) 0.2837(4) 0.2063(3) 0.0527(15) Uani 1 1 d . . . H213 H 0.3296 0.2785 0.1636 0.063 Uiso 1 1 calc R . . C214 C 0.3788(2) 0.2585(4) 0.2349(3) 0.0646(19) Uani 1 1 d . . . H214 H 0.4003 0.2353 0.2121 0.078 Uiso 1 1 calc R . . C215 C 0.3891(2) 0.2673(5) 0.2963(4) 0.076(2) Uani 1 1 d . . . H215 H 0.4179 0.2516 0.3167 0.092 Uiso 1 1 calc R . . C216 C 0.3565(2) 0.2997(5) 0.3282(3) 0.0642(18) Uani 1 1 d . . . H216 H 0.3637 0.3056 0.3710 0.077 Uiso 1 1 calc R . . N221 N 0.23860(14) 0.3949(3) 0.25035(18) 0.0399(10) Uani 1 1 d . . . N222 N 0.20173(15) 0.4254(3) 0.21428(19) 0.0440(11) Uani 1 1 d . . . C223 C 0.2019(2) 0.4008(4) 0.1555(2) 0.0545(16) Uani 1 1 d . . . H223 H 0.1794 0.4143 0.1222 0.065 Uiso 1 1 calc R . . C224 C 0.2401(2) 0.3537(4) 0.1532(2) 0.0509(15) Uani 1 1 d . . . H224 H 0.2497 0.3276 0.1185 0.061 Uiso 1 1 calc R . . C225 C 0.26258(17) 0.3516(3) 0.2136(2) 0.0371(12) Uani 1 1 d . . . C231 C 0.14401(16) 0.4246(3) 0.2811(2) 0.0364(11) Uani 1 1 d . . . C232 C 0.14486(16) 0.3298(3) 0.2823(2) 0.0366(11) Uani 1 1 d . . . H232 H 0.1626 0.2977 0.2578 0.044 Uiso 1 1 calc R . . C233 C 0.12039(15) 0.2811(3) 0.3185(2) 0.0341(11) Uani 1 1 d . . . H233 H 0.1219 0.2160 0.3193 0.041 Uiso 1 1 calc R . . C234 C 0.09348(16) 0.3270(4) 0.3539(2) 0.0344(11) Uani 1 1 d . . . C235 C 0.09338(17) 0.4215(4) 0.3533(2) 0.0417(13) Uani 1 1 d . . . H235 H 0.0758 0.4537 0.3780 0.050 Uiso 1 1 calc R . . C236 C 0.11807(17) 0.4700(4) 0.3177(2) 0.0420(12) Uani 1 1 d . . . H236 H 0.1174 0.5351 0.3180 0.050 Uiso 1 1 calc R . . C237 C 0.16908(19) 0.4790(4) 0.2397(3) 0.0493(14) Uani 1 1 d . . . H23A H 0.1475 0.5048 0.2062 0.059 Uiso 1 1 calc R . . H23B H 0.1843 0.5309 0.2628 0.059 Uiso 1 1 calc R . . C238 C 0.06595(18) 0.2768(4) 0.3947(2) 0.0430(13) Uani 1 1 d . . . H23C H 0.0786 0.2897 0.4374 0.052 Uiso 1 1 calc R . . H23D H 0.0353 0.3017 0.3875 0.052 Uiso 1 1 calc R . . N241 N 0.04028(13) 0.1393(3) 0.33598(17) 0.0317(9) Uani 1 1 d . . . N242 N 0.06376(14) 0.1786(3) 0.38605(17) 0.0387(10) Uani 1 1 d . . . C243 C 0.08251(19) 0.1135(4) 0.4250(2) 0.0524(15) Uani 1 1 d . . . H243 H 0.1007 0.1243 0.4628 0.063 Uiso 1 1 calc R . . C244 C 0.07088(19) 0.0302(4) 0.4008(3) 0.0558(16) Uani 1 1 d . . . H244 H 0.0788 -0.0282 0.4180 0.067 Uiso 1 1 calc R . . C245 C 0.04469(16) 0.0489(3) 0.3447(2) 0.0356(11) Uani 1 1 d . . . N251 N 0.0000 0.0357(4) 0.2500 0.0322(12) Uani 1 2 d S . . C252 C 0.02220(16) -0.0109(3) 0.2978(2) 0.0387(12) Uani 1 1 d . . . C253 C 0.02275(19) -0.1057(4) 0.2986(3) 0.0472(14) Uani 1 1 d . . . H253 H 0.0386 -0.1377 0.3323 0.057 Uiso 1 1 calc R . . C254 C 0.0000 -0.1532(5) 0.2500 0.054(2) Uani 1 2 d S . . H254 H 0.0000 -0.2184 0.2500 0.065 Uiso 1 2 calc SR . . N13 N 0.0384(2) 0.6756(4) 0.3455(3) 0.0730(17) Uani 1 1 d . . . C12 C 0.0446(2) 0.6547(4) 0.3943(3) 0.0630(18) Uani 1 1 d . . . C11 C 0.0537(3) 0.6243(6) 0.4573(3) 0.102(3) Uani 1 1 d . . . H11A H 0.0329 0.5752 0.4637 0.153 Uiso 1 1 calc R . . H11B H 0.0499 0.6759 0.4841 0.153 Uiso 1 1 calc R . . H11C H 0.0843 0.6013 0.4664 0.153 Uiso 1 1 calc R . . C21 C -0.0107(3) 0.8446(6) -0.0069(4) 0.105(3) Uani 1 1 d . . . H21A H -0.0391 0.8299 0.0064 0.158 Uiso 1 1 calc R . . H21B H 0.0039 0.7878 -0.0165 0.158 Uiso 1 1 calc R . . H21C H -0.0161 0.8835 -0.0430 0.158 Uiso 1 1 calc R . . C22 C 0.0178(3) 0.8928(6) 0.0412(4) 0.089(2) Uani 1 1 d . . . N23 N 0.0396(3) 0.9305(7) 0.0774(4) 0.141(4) Uani 1 1 d . . . P1 P 0.15921(5) 0.85001(10) 0.48449(6) 0.0460(4) Uani 1 1 d . . . F11 F 0.20321(14) 0.8129(3) 0.46460(19) 0.0888(13) Uani 1 1 d . . . F12 F 0.17599(18) 0.9500(3) 0.4799(2) 0.1100(17) Uani 1 1 d . . . F13 F 0.11447(14) 0.8865(3) 0.50444(16) 0.0826(13) Uani 1 1 d . . . F14 F 0.14093(16) 0.7496(3) 0.4890(2) 0.1063(16) Uani 1 1 d . . . F15 F 0.18059(13) 0.8426(3) 0.55301(16) 0.0824(13) Uani 1 1 d . . . F16 F 0.13626(16) 0.8566(4) 0.41612(17) 0.1010(16) Uani 1 1 d . . . P2 P 0.08648(7) 0.58812(12) 0.06836(7) 0.0618(5) Uani 1 1 d D . . F21 F 0.04349(13) 0.5244(3) 0.06870(19) 0.0849(12) Uani 1 1 d . A . F22 F 0.0884(3) 0.5882(5) -0.0011(3) 0.071(2) Uiso 0.575(10) 1 d PDU A 1 F22' F 0.0605(4) 0.5875(7) -0.0031(4) 0.081(3) Uiso 0.425(10) 1 d PDU A 2 F23 F 0.11547(14) 0.4967(3) 0.0659(2) 0.0855(13) Uani 1 1 d . A . F24 F 0.1367(2) 0.6413(5) 0.0790(3) 0.066(2) Uiso 0.575(10) 1 d PDU A 1 F24' F 0.1177(4) 0.6611(6) 0.0524(5) 0.072(3) Uiso 0.425(10) 1 d PDU A 2 F25 F 0.09399(15) 0.5829(3) 0.13844(17) 0.0840(12) Uani 1 1 d . A . F26 F 0.0590(2) 0.6783(3) 0.0720(2) 0.1148(18) Uani 1 1 d . A . 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 Cu1 0.0488(4) 0.0669(5) 0.0360(4) -0.0017(3) 0.0188(3) -0.0018(3) Cu2 0.0330(4) 0.0249(4) 0.0261(4) 0.000 0.0063(3) 0.000 N111 0.045(3) 0.041(3) 0.038(2) -0.0044(19) 0.0123(19) -0.006(2) C112 0.038(3) 0.038(3) 0.025(2) 0.001(2) 0.000(2) 0.000(2) C113 0.043(3) 0.045(3) 0.035(3) -0.003(2) 0.008(2) 0.003(2) C114 0.064(4) 0.051(4) 0.050(3) -0.009(3) 0.008(3) 0.013(3) C115 0.073(4) 0.034(3) 0.066(4) -0.010(3) 0.006(3) -0.003(3) C116 0.067(4) 0.046(4) 0.053(3) 0.001(3) 0.013(3) -0.020(3) N121 0.036(2) 0.034(2) 0.0278(19) -0.0009(17) 0.0024(17) -0.0001(18) N122 0.042(2) 0.034(2) 0.032(2) -0.0003(18) 0.0017(18) 0.0039(19) C123 0.046(3) 0.040(3) 0.035(3) 0.003(2) 0.004(2) -0.003(2) C124 0.037(3) 0.046(3) 0.029(2) 0.000(2) 0.009(2) 0.000(2) C125 0.030(3) 0.038(3) 0.028(2) -0.001(2) 0.0031(19) 0.001(2) C131 0.036(3) 0.026(3) 0.037(2) -0.005(2) 0.009(2) 0.006(2) C132 0.050(3) 0.030(3) 0.042(3) -0.001(2) 0.013(2) 0.007(2) C133 0.042(3) 0.031(3) 0.043(3) -0.008(2) 0.012(2) -0.005(2) C134 0.034(3) 0.028(3) 0.039(3) -0.009(2) 0.012(2) 0.007(2) C135 0.040(3) 0.036(3) 0.037(3) 0.000(2) 0.012(2) 0.005(2) C136 0.041(3) 0.030(3) 0.040(3) -0.008(2) 0.015(2) -0.004(2) C137 0.045(3) 0.037(3) 0.044(3) -0.006(2) 0.002(2) 0.010(2) C138 0.045(3) 0.037(3) 0.035(3) -0.010(2) 0.008(2) 0.003(2) N141 0.029(2) 0.034(2) 0.0268(19) -0.0047(16) 0.0054(16) 0.0002(17) N142 0.037(2) 0.038(2) 0.0258(19) -0.0066(17) 0.0102(17) 0.0019(18) C143 0.053(3) 0.053(3) 0.029(2) -0.001(2) 0.021(2) 0.005(3) C144 0.040(3) 0.040(3) 0.031(2) 0.004(2) 0.011(2) -0.001(2) C145 0.030(2) 0.030(2) 0.027(2) 0.0011(19) 0.0060(19) -0.0016(19) N151 0.028(3) 0.033(3) 0.024(3) 0.000 0.008(2) 0.000 C152 0.031(2) 0.030(3) 0.023(2) 0.0010(18) 0.0023(18) -0.0032(19) C153 0.037(3) 0.031(3) 0.033(2) 0.004(2) 0.007(2) -0.003(2) C154 0.046(4) 0.025(4) 0.035(4) 0.000 0.003(3) 0.000 N211 0.040(3) 0.056(3) 0.046(3) 0.014(2) 0.016(2) 0.003(2) C212 0.049(3) 0.033(3) 0.043(3) 0.001(2) 0.023(2) -0.008(2) C213 0.063(4) 0.042(3) 0.063(4) -0.001(3) 0.037(3) -0.005(3) C214 0.060(4) 0.051(4) 0.093(5) 0.012(4) 0.045(4) 0.006(3) C215 0.054(4) 0.085(5) 0.095(6) 0.034(4) 0.028(4) 0.014(4) C216 0.047(4) 0.085(5) 0.064(4) 0.023(4) 0.018(3) 0.009(3) N221 0.041(3) 0.043(3) 0.038(2) 0.0054(19) 0.014(2) -0.002(2) N222 0.048(3) 0.047(3) 0.039(2) 0.009(2) 0.010(2) -0.004(2) C223 0.061(4) 0.062(4) 0.040(3) 0.009(3) 0.008(3) -0.021(3) C224 0.063(4) 0.056(4) 0.039(3) -0.004(3) 0.024(3) -0.015(3) C225 0.043(3) 0.037(3) 0.034(2) 0.001(2) 0.015(2) -0.010(2) C231 0.033(3) 0.038(3) 0.037(3) 0.001(2) 0.002(2) -0.002(2) C232 0.033(3) 0.039(3) 0.039(3) -0.005(2) 0.010(2) 0.003(2) C233 0.034(3) 0.034(3) 0.033(2) -0.003(2) 0.001(2) -0.001(2) C234 0.034(3) 0.042(3) 0.026(2) -0.005(2) 0.002(2) -0.006(2) C235 0.040(3) 0.047(3) 0.037(3) -0.010(2) 0.007(2) 0.005(2) C236 0.040(3) 0.037(3) 0.049(3) -0.006(2) 0.006(2) 0.004(2) C237 0.048(3) 0.045(3) 0.055(3) 0.010(3) 0.008(3) 0.004(3) C238 0.042(3) 0.053(4) 0.034(3) -0.009(2) 0.007(2) -0.005(3) N241 0.031(2) 0.033(2) 0.032(2) 0.0022(17) 0.0061(16) -0.0008(17) N242 0.039(2) 0.050(3) 0.027(2) 0.0047(19) 0.0057(18) -0.006(2) C243 0.047(3) 0.068(4) 0.040(3) 0.020(3) -0.001(3) -0.009(3) C244 0.048(3) 0.056(4) 0.061(4) 0.031(3) 0.004(3) 0.000(3) C245 0.035(3) 0.035(3) 0.039(3) 0.009(2) 0.012(2) 0.001(2) N251 0.033(3) 0.028(3) 0.038(3) 0.000 0.013(2) 0.000 C252 0.036(3) 0.031(3) 0.052(3) 0.007(2) 0.019(2) 0.000(2) C253 0.048(3) 0.034(3) 0.065(4) 0.013(3) 0.029(3) 0.008(2) C254 0.069(6) 0.026(4) 0.078(6) 0.000 0.041(5) 0.000 N13 0.104(5) 0.051(3) 0.068(4) 0.009(3) 0.028(3) -0.008(3) C12 0.085(5) 0.043(4) 0.063(4) 0.006(3) 0.017(4) -0.013(3) C11 0.123(8) 0.111(7) 0.065(5) 0.014(5) -0.008(5) -0.040(6) C21 0.090(6) 0.103(7) 0.121(8) -0.028(6) 0.011(6) -0.009(5) C22 0.084(6) 0.092(6) 0.089(6) -0.029(5) 0.012(5) -0.011(5) N23 0.140(8) 0.150(9) 0.122(7) -0.047(6) -0.009(6) -0.044(6) P1 0.0593(10) 0.0431(9) 0.0399(7) 0.0060(6) 0.0207(7) 0.0039(7) F11 0.078(3) 0.110(4) 0.090(3) 0.007(3) 0.046(2) 0.017(2) F12 0.157(5) 0.057(3) 0.122(4) 0.025(3) 0.040(3) -0.025(3) F13 0.090(3) 0.104(3) 0.061(2) 0.029(2) 0.033(2) 0.045(2) F14 0.108(4) 0.057(3) 0.160(5) -0.008(3) 0.041(3) -0.014(2) F15 0.068(3) 0.131(4) 0.049(2) 0.026(2) 0.0104(18) -0.004(2) F16 0.111(4) 0.149(5) 0.043(2) -0.011(2) 0.014(2) 0.028(3) P2 0.0949(14) 0.0477(10) 0.0495(9) 0.0105(7) 0.0323(9) 0.0057(9) F21 0.072(3) 0.086(3) 0.095(3) -0.009(2) 0.008(2) 0.011(2) F23 0.084(3) 0.060(3) 0.123(4) 0.005(2) 0.052(3) 0.006(2) F25 0.109(3) 0.084(3) 0.061(2) 0.009(2) 0.018(2) -0.003(2) F26 0.173(5) 0.062(3) 0.104(4) 0.007(2) 0.005(3) 0.048(3) _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 Cu1 N211 1.987(4) . ? Cu1 N111 2.008(4) . ? Cu1 N121 2.140(4) . ? Cu1 N221 2.158(4) . ? Cu2 N251 1.951(5) . ? Cu2 N151 1.952(5) . ? Cu2 N241 2.157(4) 2 ? Cu2 N241 2.157(4) . ? Cu2 N141 2.349(4) 2 ? Cu2 N141 2.349(4) . ? N111 C116 1.337(7) . ? N111 C112 1.355(6) . ? C112 C113 1.378(7) . ? C112 C125 1.455(7) . ? C113 C114 1.360(8) . ? C114 C115 1.369(9) . ? C115 C116 1.392(8) . ? N121 N122 1.348(5) . ? N121 C125 1.352(6) . ? N122 C123 1.347(6) . ? N122 C137 1.459(6) . ? C123 C124 1.357(7) . ? C124 C125 1.402(7) . ? C131 C132 1.382(7) . ? C131 C136 1.394(7) . ? C131 C137 1.515(7) . ? C132 C133 1.395(7) . ? C133 C134 1.379(7) . ? C134 C135 1.386(7) . ? C134 C138 1.520(7) . ? C135 C136 1.378(7) . ? C138 N142 1.468(6) . ? N141 C145 1.340(6) . ? N141 N142 1.350(5) . ? N142 C143 1.341(6) . ? C143 C144 1.372(7) . ? C144 C145 1.395(6) . ? C145 C152 1.461(6) . ? N151 C152 1.363(5) 2 ? N151 C152 1.363(5) . ? C152 C153 1.390(6) . ? C153 C154 1.378(6) . ? C154 C153 1.378(6) 2 ? N211 C216 1.336(7) . ? N211 C212 1.368(7) . ? C212 C213 1.378(7) . ? C212 C225 1.457(7) . ? C213 C214 1.380(9) . ? C214 C215 1.364(10) . ? C215 C216 1.391(9) . ? N221 C225 1.337(6) . ? N221 N222 1.350(6) . ? N222 C223 1.361(7) . ? N222 C237 1.448(7) . ? C223 C224 1.358(9) . ? C224 C225 1.415(7) . ? C231 C232 1.383(7) . ? C231 C236 1.389(7) . ? C231 C237 1.511(7) . ? C232 C233 1.379(7) . ? C233 C234 1.395(7) . ? C234 C235 1.379(7) . ? C234 C238 1.517(7) . ? C235 C236 1.372(7) . ? C238 N242 1.446(7) . ? N241 C245 1.337(6) . ? N241 N242 1.357(5) . ? N242 C243 1.352(7) . ? C243 C244 1.354(9) . ? C244 C245 1.402(7) . ? C245 C252 1.452(7) . ? N251 C252 1.354(6) 2 ? N251 C252 1.354(6) . ? C252 C253 1.384(7) . ? C253 C254 1.381(7) . ? C254 C253 1.381(7) 2 ? N13 C12 1.121(8) . ? C12 C11 1.461(9) . ? C21 C22 1.453(11) . ? C22 N23 1.108(10) . ? P1 F12 1.554(4) . ? P1 F11 1.569(4) . ? P1 F15 1.571(4) . ? P1 F14 1.576(4) . ? P1 F16 1.581(4) . ? P1 F13 1.588(4) . ? P2 F24' 1.504(8) . ? P2 F25 1.549(4) . ? P2 F22 1.563(6) . ? P2 F26 1.568(5) . ? P2 F23 1.604(4) . ? P2 F21 1.605(5) . ? P2 F22' 1.667(9) . ? P2 F24 1.696(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 N211 Cu1 N111 149.55(19) . . ? N211 Cu1 N121 121.43(17) . . ? N111 Cu1 N121 80.28(16) . . ? N211 Cu1 N221 79.58(17) . . ? N111 Cu1 N221 107.62(17) . . ? N121 Cu1 N221 122.98(15) . . ? N251 Cu2 N151 180.000(1) . . ? N251 Cu2 N241 78.26(11) . 2 ? N151 Cu2 N241 101.74(11) . 2 ? N251 Cu2 N241 78.26(11) . . ? N151 Cu2 N241 101.74(11) . . ? N241 Cu2 N241 156.5(2) 2 . ? N251 Cu2 N141 102.77(10) . 2 ? N151 Cu2 N141 77.23(10) . 2 ? N241 Cu2 N141 99.29(13) 2 2 ? N241 Cu2 N141 85.91(13) . 2 ? N251 Cu2 N141 102.77(10) . . ? N151 Cu2 N141 77.23(10) . . ? N241 Cu2 N141 85.91(13) 2 . ? N241 Cu2 N141 99.29(13) . . ? N141 Cu2 N141 154.46(19) 2 . ? C116 N111 C112 117.7(5) . . ? C116 N111 Cu1 126.0(4) . . ? C112 N111 Cu1 115.9(3) . . ? N111 C112 C113 121.9(5) . . ? N111 C112 C125 115.1(4) . . ? C113 C112 C125 122.9(5) . . ? C114 C113 C112 119.7(5) . . ? C113 C114 C115 119.5(5) . . ? C114 C115 C116 118.5(6) . . ? N111 C116 C115 122.6(5) . . ? N122 N121 C125 105.1(4) . . ? N122 N121 Cu1 144.6(3) . . ? C125 N121 Cu1 110.0(3) . . ? C123 N122 N121 111.5(4) . . ? C123 N122 C137 127.8(5) . . ? N121 N122 C137 120.3(4) . . ? N122 C123 C124 107.9(5) . . ? C123 C124 C125 105.4(4) . . ? N121 C125 C124 110.1(4) . . ? N121 C125 C112 118.4(4) . . ? C124 C125 C112 131.5(4) . . ? C132 C131 C136 117.9(5) . . ? C132 C131 C137 121.0(5) . . ? C136 C131 C137 120.9(5) . . ? C131 C132 C133 121.2(5) . . ? C134 C133 C132 119.8(5) . . ? C133 C134 C135 119.5(5) . . ? C133 C134 C138 120.7(5) . . ? C135 C134 C138 119.8(4) . . ? C136 C135 C134 120.1(5) . . ? C135 C136 C131 121.2(5) . . ? N122 C137 C131 110.3(4) . . ? N142 C138 C134 110.8(4) . . ? C145 N141 N142 104.5(4) . . ? C145 N141 Cu2 105.5(3) . . ? N142 N141 Cu2 146.0(3) . . ? C143 N142 N141 111.6(4) . . ? C143 N142 C138 126.5(4) . . ? N141 N142 C138 121.0(4) . . ? N142 C143 C144 108.1(4) . . ? C143 C144 C145 103.9(4) . . ? N141 C145 C144 111.9(4) . . ? N141 C145 C152 118.6(4) . . ? C144 C145 C152 129.5(4) . . ? C152 N151 C152 119.4(6) 2 . ? C152 N151 Cu2 120.3(3) 2 . ? C152 N151 Cu2 120.3(3) . . ? N151 C152 C153 121.2(4) . . ? N151 C152 C145 115.5(4) . . ? C153 C152 C145 123.3(4) . . ? C154 C153 C152 118.4(5) . . ? C153 C154 C153 121.1(6) 2 . ? C216 N211 C212 117.5(5) . . ? C216 N211 Cu1 127.0(4) . . ? C212 N211 Cu1 115.5(4) . . ? N211 C212 C213 121.6(5) . . ? N211 C212 C225 114.7(4) . . ? C213 C212 C225 123.6(5) . . ? C212 C213 C214 119.7(6) . . ? C215 C214 C213 119.3(6) . . ? C214 C215 C216 118.7(7) . . ? N211 C216 C215 123.2(7) . . ? C225 N221 N222 105.6(4) . . ? C225 N221 Cu1 108.8(3) . . ? N222 N221 Cu1 143.0(3) . . ? N221 N222 C223 111.3(5) . . ? N221 N222 C237 120.0(4) . . ? C223 N222 C237 128.8(5) . . ? C224 C223 N222 107.5(5) . . ? C223 C224 C225 105.3(5) . . ? N221 C225 C224 110.3(5) . . ? N221 C225 C212 117.7(4) . . ? C224 C225 C212 131.9(5) . . ? C232 C231 C236 118.4(5) . . ? C232 C231 C237 121.9(5) . . ? C236 C231 C237 119.7(5) . . ? C233 C232 C231 121.1(5) . . ? C232 C233 C234 120.2(5) . . ? C235 C234 C233 118.3(5) . . ? C235 C234 C238 119.3(4) . . ? C233 C234 C238 122.4(5) . . ? C236 C235 C234 121.4(5) . . ? C235 C236 C231 120.5(5) . . ? N222 C237 C231 113.4(4) . . ? N242 C238 C234 114.6(4) . . ? C245 N241 N242 105.5(4) . . ? C245 N241 Cu2 111.2(3) . . ? N242 N241 Cu2 143.3(3) . . ? C243 N242 N241 110.4(5) . . ? C243 N242 C238 127.2(5) . . ? N241 N242 C238 122.4(4) . . ? N242 C243 C244 108.4(5) . . ? C243 C244 C245 105.0(5) . . ? N241 C245 C244 110.7(5) . . ? N241 C245 C252 117.5(4) . . ? C244 C245 C252 131.8(5) . . ? C252 N251 C252 119.7(6) 2 . ? C252 N251 Cu2 120.1(3) 2 . ? C252 N251 Cu2 120.1(3) . . ? N251 C252 C253 121.1(5) . . ? N251 C252 C245 112.9(4) . . ? C253 C252 C245 126.0(5) . . ? C254 C253 C252 119.2(6) . . ? C253 C254 C253 119.7(7) 2 . ? N13 C12 C11 177.7(9) . . ? N23 C22 C21 179.1(12) . . ? F12 P1 F11 90.1(3) . . ? F12 P1 F15 92.2(3) . . ? F11 P1 F15 90.6(2) . . ? F12 P1 F14 178.5(3) . . ? F11 P1 F14 91.3(3) . . ? F15 P1 F14 88.3(3) . . ? F12 P1 F16 88.9(3) . . ? F11 P1 F16 90.8(2) . . ? F15 P1 F16 178.2(3) . . ? F14 P1 F16 90.7(3) . . ? F12 P1 F13 90.4(3) . . ? F11 P1 F13 179.4(3) . . ? F15 P1 F13 89.5(2) . . ? F14 P1 F13 88.2(3) . . ? F16 P1 F13 89.0(2) . . ? F24' P2 F25 105.9(5) . . ? F24' P2 F22 69.0(5) . . ? F25 P2 F22 169.2(4) . . ? F24' P2 F26 77.2(5) . . ? F25 P2 F26 89.1(3) . . ? F22 P2 F26 98.8(3) . . ? F24' P2 F23 102.2(4) . . ? F25 P2 F23 89.9(2) . . ? F22 P2 F23 82.1(3) . . ? F26 P2 F23 178.6(3) . . ? F24' P2 F21 162.7(5) . . ? F25 P2 F21 87.6(2) . . ? F22 P2 F21 99.3(4) . . ? F26 P2 F21 92.6(3) . . ? F23 P2 F21 88.3(2) . . ? F24' P2 F22' 90.0(5) . . ? F25 P2 F22' 160.3(5) . . ? F22 P2 F22' 30.0(4) . . ? F26 P2 F22' 83.0(4) . . ? F23 P2 F22' 98.3(4) . . ? F21 P2 F22' 74.7(5) . . ? F24' P2 F24 28.7(4) . . ? F25 P2 F24 83.8(3) . . ? F22 P2 F24 88.1(4) . . ? F26 P2 F24 94.8(4) . . ? F23 P2 F24 84.1(3) . . ? F21 P2 F24 168.6(3) . . ? F22' P2 F24 114.7(5) . . ? 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 Cu1 N111 C116 44.7(6) . . . . ? N121 Cu1 N111 C116 -176.5(5) . . . . ? N221 Cu1 N111 C116 -54.8(5) . . . . ? N211 Cu1 N111 C112 -142.3(4) . . . . ? N121 Cu1 N111 C112 -3.5(3) . . . . ? N221 Cu1 N111 C112 118.2(3) . . . . ? C116 N111 C112 C113 -0.3(7) . . . . ? Cu1 N111 C112 C113 -173.9(4) . . . . ? C116 N111 C112 C125 179.1(5) . . . . ? Cu1 N111 C112 C125 5.5(5) . . . . ? N111 C112 C113 C114 -0.1(8) . . . . ? C125 C112 C113 C114 -179.5(5) . . . . ? C112 C113 C114 C115 1.3(8) . . . . ? C113 C114 C115 C116 -1.9(9) . . . . ? C112 N111 C116 C115 -0.4(8) . . . . ? Cu1 N111 C116 C115 172.5(4) . . . . ? C114 C115 C116 N111 1.5(9) . . . . ? N211 Cu1 N121 N122 -14.4(6) . . . . ? N111 Cu1 N121 N122 -171.3(5) . . . . ? N221 Cu1 N121 N122 83.9(5) . . . . ? N211 Cu1 N121 C125 157.8(3) . . . . ? N111 Cu1 N121 C125 0.8(3) . . . . ? N221 Cu1 N121 C125 -103.9(3) . . . . ? C125 N121 N122 C123 1.7(5) . . . . ? Cu1 N121 N122 C123 174.1(4) . . . . ? C125 N121 N122 C137 174.9(4) . . . . ? Cu1 N121 N122 C137 -12.8(8) . . . . ? N121 N122 C123 C124 -1.1(6) . . . . ? C137 N122 C123 C124 -173.7(4) . . . . ? N122 C123 C124 C125 0.1(6) . . . . ? N122 N121 C125 C124 -1.6(5) . . . . ? Cu1 N121 C125 C124 -176.9(3) . . . . ? N122 N121 C125 C112 177.1(4) . . . . ? Cu1 N121 C125 C112 1.8(5) . . . . ? C123 C124 C125 N121 0.9(5) . . . . ? C123 C124 C125 C112 -177.5(5) . . . . ? N111 C112 C125 N121 -4.8(6) . . . . ? C113 C112 C125 N121 174.6(4) . . . . ? N111 C112 C125 C124 173.5(5) . . . . ? C113 C112 C125 C124 -7.1(8) . . . . ? C136 C131 C132 C133 -3.0(7) . . . . ? C137 C131 C132 C133 172.0(4) . . . . ? C131 C132 C133 C134 -0.6(7) . . . . ? C132 C133 C134 C135 4.3(7) . . . . ? C132 C133 C134 C138 -173.5(4) . . . . ? C133 C134 C135 C136 -4.4(7) . . . . ? C138 C134 C135 C136 173.4(4) . . . . ? C134 C135 C136 C131 0.7(7) . . . . ? C132 C131 C136 C135 3.0(7) . . . . ? C137 C131 C136 C135 -172.0(4) . . . . ? C123 N122 C137 C131 90.1(6) . . . . ? N121 N122 C137 C131 -81.8(6) . . . . ? C132 C131 C137 N122 -78.7(6) . . . . ? C136 C131 C137 N122 96.1(6) . . . . ? C133 C134 C138 N142 112.0(5) . . . . ? C135 C134 C138 N142 -65.7(6) . . . . ? N251 Cu2 N141 C145 165.9(3) . . . . ? N151 Cu2 N141 C145 -14.1(3) . . . . ? N241 Cu2 N141 C145 89.0(3) 2 . . . ? N241 Cu2 N141 C145 -114.1(3) . . . . ? N141 Cu2 N141 C145 -14.1(3) 2 . . . ? N251 Cu2 N141 N142 14.8(5) . . . . ? N151 Cu2 N141 N142 -165.2(5) . . . . ? N241 Cu2 N141 N142 -62.2(5) 2 . . . ? N241 Cu2 N141 N142 94.8(5) . . . . ? N141 Cu2 N141 N142 -165.2(5) 2 . . . ? C145 N141 N142 C143 0.7(5) . . . . ? Cu2 N141 N142 C143 152.0(4) . . . . ? C145 N141 N142 C138 170.4(4) . . . . ? Cu2 N141 N142 C138 -38.3(7) . . . . ? C134 C138 N142 C143 91.2(6) . . . . ? C134 C138 N142 N141 -76.9(5) . . . . ? N141 N142 C143 C144 -1.2(6) . . . . ? C138 N142 C143 C144 -170.2(4) . . . . ? N142 C143 C144 C145 1.1(6) . . . . ? N142 N141 C145 C144 0.0(5) . . . . ? Cu2 N141 C145 C144 -163.8(3) . . . . ? N142 N141 C145 C152 -178.5(4) . . . . ? Cu2 N141 C145 C152 17.6(5) . . . . ? C143 C144 C145 N141 -0.7(6) . . . . ? C143 C144 C145 C152 177.7(5) . . . . ? N251 Cu2 N151 C152 42(100) . . . 2 ? N241 Cu2 N151 C152 105.8(2) 2 . . 2 ? N241 Cu2 N151 C152 -74.2(2) . . . 2 ? N141 Cu2 N151 C152 8.8(2) 2 . . 2 ? N141 Cu2 N151 C152 -171.2(2) . . . 2 ? N251 Cu2 N151 C152 -138(100) . . . . ? N241 Cu2 N151 C152 -74.2(2) 2 . . . ? N241 Cu2 N151 C152 105.8(2) . . . . ? N141 Cu2 N151 C152 -171.2(2) 2 . . . ? N141 Cu2 N151 C152 8.8(2) . . . . ? C152 N151 C152 C153 -1.9(3) 2 . . . ? Cu2 N151 C152 C153 178.1(3) . . . . ? C152 N151 C152 C145 177.8(4) 2 . . . ? Cu2 N151 C152 C145 -2.2(4) . . . . ? N141 C145 C152 N151 -12.6(6) . . . . ? C144 C145 C152 N151 169.1(4) . . . . ? N141 C145 C152 C153 167.0(4) . . . . ? C144 C145 C152 C153 -11.3(8) . . . . ? N151 C152 C153 C154 3.7(6) . . . . ? C145 C152 C153 C154 -175.9(4) . . . . ? C152 C153 C154 C153 -1.8(3) . . . 2 ? N111 Cu1 N211 C216 62.1(7) . . . . ? N121 Cu1 N211 C216 -68.4(6) . . . . ? N221 Cu1 N211 C216 169.2(6) . . . . ? N111 Cu1 N211 C212 -121.5(4) . . . . ? N121 Cu1 N211 C212 108.1(4) . . . . ? N221 Cu1 N211 C212 -14.3(4) . . . . ? C216 N211 C212 C213 2.6(8) . . . . ? Cu1 N211 C212 C213 -174.2(4) . . . . ? C216 N211 C212 C225 -174.0(5) . . . . ? Cu1 N211 C212 C225 9.2(6) . . . . ? N211 C212 C213 C214 -1.4(8) . . . . ? C225 C212 C213 C214 174.8(5) . . . . ? C212 C213 C214 C215 -0.6(9) . . . . ? C213 C214 C215 C216 1.4(10) . . . . ? C212 N211 C216 C215 -1.8(9) . . . . ? Cu1 N211 C216 C215 174.6(5) . . . . ? C214 C215 C216 N211 -0.1(11) . . . . ? N211 Cu1 N221 C225 17.3(3) . . . . ? N111 Cu1 N221 C225 166.7(3) . . . . ? N121 Cu1 N221 C225 -103.6(3) . . . . ? N211 Cu1 N221 N222 174.7(6) . . . . ? N111 Cu1 N221 N222 -35.9(6) . . . . ? N121 Cu1 N221 N222 53.8(6) . . . . ? C225 N221 N222 C223 0.8(6) . . . . ? Cu1 N221 N222 C223 -157.0(5) . . . . ? C225 N221 N222 C237 -177.6(4) . . . . ? Cu1 N221 N222 C237 24.6(8) . . . . ? N221 N222 C223 C224 -0.5(6) . . . . ? C237 N222 C223 C224 177.7(5) . . . . ? N222 C223 C224 C225 -0.1(6) . . . . ? N222 N221 C225 C224 -0.8(5) . . . . ? Cu1 N221 C225 C224 165.3(3) . . . . ? N222 N221 C225 C212 176.0(4) . . . . ? Cu1 N221 C225 C212 -17.9(5) . . . . ? C223 C224 C225 N221 0.6(6) . . . . ? C223 C224 C225 C212 -175.7(5) . . . . ? N211 C212 C225 N221 7.1(7) . . . . ? C213 C212 C225 N221 -169.4(5) . . . . ? N211 C212 C225 C224 -176.8(5) . . . . ? C213 C212 C225 C224 6.7(9) . . . . ? C236 C231 C232 C233 0.5(7) . . . . ? C237 C231 C232 C233 -177.4(5) . . . . ? C231 C232 C233 C234 1.2(7) . . . . ? C232 C233 C234 C235 -2.3(7) . . . . ? C232 C233 C234 C238 -179.9(4) . . . . ? C233 C234 C235 C236 1.7(7) . . . . ? C238 C234 C235 C236 179.3(5) . . . . ? C234 C235 C236 C231 0.0(8) . . . . ? C232 C231 C236 C235 -1.1(7) . . . . ? C237 C231 C236 C235 176.8(5) . . . . ? N221 N222 C237 C231 -68.9(6) . . . . ? C223 N222 C237 C231 113.1(6) . . . . ? C232 C231 C237 N222 -14.6(7) . . . . ? C236 C231 C237 N222 167.6(5) . . . . ? C235 C234 C238 N242 172.2(4) . . . . ? C233 C234 C238 N242 -10.2(7) . . . . ? N251 Cu2 N241 C245 0.4(3) . . . . ? N151 Cu2 N241 C245 -179.6(3) . . . . ? N241 Cu2 N241 C245 0.4(3) 2 . . . ? N141 Cu2 N241 C245 104.4(3) 2 . . . ? N141 Cu2 N241 C245 -100.8(3) . . . . ? N251 Cu2 N241 N242 179.9(5) . . . . ? N151 Cu2 N241 N242 -0.1(5) . . . . ? N241 Cu2 N241 N242 179.9(5) 2 . . . ? N141 Cu2 N241 N242 -76.1(5) 2 . . . ? N141 Cu2 N241 N242 78.7(5) . . . . ? C245 N241 N242 C243 0.3(5) . . . . ? Cu2 N241 N242 C243 -179.3(4) . . . . ? C245 N241 N242 C238 -178.0(4) . . . . ? Cu2 N241 N242 C238 2.4(8) . . . . ? C234 C238 N242 C243 110.7(6) . . . . ? C234 C238 N242 N241 -71.3(6) . . . . ? N241 N242 C243 C244 -0.8(6) . . . . ? C238 N242 C243 C244 177.4(5) . . . . ? N242 C243 C244 C245 0.9(7) . . . . ? N242 N241 C245 C244 0.3(5) . . . . ? Cu2 N241 C245 C244 -179.9(3) . . . . ? N242 N241 C245 C252 179.4(4) . . . . ? Cu2 N241 C245 C252 -0.9(5) . . . . ? C243 C244 C245 N241 -0.8(6) . . . . ? C243 C244 C245 C252 -179.6(5) . . . . ? N151 Cu2 N251 C252 64(100) . . . 2 ? N241 Cu2 N251 C252 0.2(3) 2 . . 2 ? N241 Cu2 N251 C252 -179.8(3) . . . 2 ? N141 Cu2 N251 C252 97.2(2) 2 . . 2 ? N141 Cu2 N251 C252 -82.8(2) . . . 2 ? N151 Cu2 N251 C252 -116(100) . . . . ? N241 Cu2 N251 C252 -179.8(3) 2 . . . ? N241 Cu2 N251 C252 0.2(3) . . . . ? N141 Cu2 N251 C252 -82.8(2) 2 . . . ? N141 Cu2 N251 C252 97.2(2) . . . . ? C252 N251 C252 C253 0.2(3) 2 . . . ? Cu2 N251 C252 C253 -179.8(3) . . . . ? C252 N251 C252 C245 179.2(5) 2 . . . ? Cu2 N251 C252 C245 -0.8(5) . . . . ? N241 C245 C252 N251 1.1(6) . . . . ? C244 C245 C252 N251 179.9(5) . . . . ? N241 C245 C252 C253 -179.9(5) . . . . ? C244 C245 C252 C253 -1.1(9) . . . . ? N251 C252 C253 C254 -0.4(7) . . . . ? C245 C252 C253 C254 -179.3(4) . . . . ? C252 C253 C254 C253 0.2(3) . . . 2 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.733 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.096 #===END data_Cu222 _database_code_depnum_ccdc_archive 'CCDC 265433' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C90 H76 Cu3 N22 O4, 2(C2 H3 N), 4(F6 P)' _chemical_formula_sum 'C94 H82 Cu3 F24 N24 O4 P4' _chemical_formula_weight 2382.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.397(3) _cell_length_b 15.0598(19) _cell_length_c 30.411(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.856(3) _cell_angle_gamma 90.00 _cell_volume 10106(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5103 _cell_measurement_theta_min 4.453 _cell_measurement_theta_max 50.749 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4836 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7357 _exptl_absorpt_correction_T_max 0.9245 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 56428 _diffrn_reflns_av_R_equivalents 0.1498 _diffrn_reflns_av_sigmaI/netI 0.1557 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.67 _reflns_number_total 11549 _reflns_number_gt 5528 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+25.9400P] 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 11549 _refine_ls_number_parameters 687 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1855 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2689 _refine_ls_wR_factor_gt 0.2079 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.034 _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 Cu1 Cu 0.5000 0.83678(7) 0.7500 0.0257(3) Uani 1 2 d S . . Cu2 Cu 0.38845(3) 0.67412(5) 0.47085(3) 0.0290(2) Uani 1 1 d . . . N111 N 0.4370(2) 0.7386(4) 0.43104(17) 0.0326(12) Uani 1 1 d . . . C112 C 0.4982(3) 0.7280(4) 0.4388(2) 0.0313(14) Uani 1 1 d . . . C113 C 0.5339(3) 0.7584(5) 0.4098(2) 0.0474(19) Uani 1 1 d . . . H113 H 0.5766 0.7514 0.4165 0.057 Uiso 1 1 calc R . . C114 C 0.5077(4) 0.7989(6) 0.3711(3) 0.065(2) Uani 1 1 d . . . H114 H 0.5322 0.8189 0.3505 0.077 Uiso 1 1 calc R . . C115 C 0.4451(4) 0.8111(6) 0.3619(3) 0.060(2) Uani 1 1 d . . . H115 H 0.4259 0.8394 0.3353 0.072 Uiso 1 1 calc R . . C116 C 0.4124(3) 0.7806(4) 0.3928(2) 0.0384(16) Uani 1 1 d . . . H116 H 0.3697 0.7893 0.3871 0.046 Uiso 1 1 calc R . . N121 N 0.4854(2) 0.6367(3) 0.50138(17) 0.0276(11) Uani 1 1 d . . . N122 N 0.5213(2) 0.6003(3) 0.53699(17) 0.0304(12) Uani 1 1 d . . . C123 C 0.5797(3) 0.6250(4) 0.5387(2) 0.0350(15) Uani 1 1 d . . . H123 H 0.6126 0.6087 0.5613 0.042 Uiso 1 1 calc R . . C124 C 0.5831(3) 0.6766(4) 0.5029(2) 0.0338(15) Uani 1 1 d . . . H124 H 0.6181 0.7035 0.4950 0.041 Uiso 1 1 calc R . . C125 C 0.5233(3) 0.6816(4) 0.4801(2) 0.0311(14) Uani 1 1 d . . . C131 C 0.4619(3) 0.5957(4) 0.5988(2) 0.0299(14) Uani 1 1 d . . . C132 C 0.4293(3) 0.5484(4) 0.6258(2) 0.0374(16) Uani 1 1 d . . . H132 H 0.4290 0.4854 0.6251 0.045 Uiso 1 1 calc R . . C133 C 0.3971(3) 0.5940(5) 0.6539(2) 0.0373(16) Uani 1 1 d . . . H133 H 0.3751 0.5616 0.6727 0.045 Uiso 1 1 calc R . . C134 C 0.3966(3) 0.6859(4) 0.6548(2) 0.0286(14) Uani 1 1 d . . . C135 C 0.4303(3) 0.7316(4) 0.62882(19) 0.0278(14) Uani 1 1 d . . . H135 H 0.4312 0.7946 0.6301 0.033 Uiso 1 1 calc R . . C136 C 0.4629(3) 0.6884(4) 0.6010(2) 0.0288(14) Uani 1 1 d . . . H136 H 0.4860 0.7214 0.5832 0.035 Uiso 1 1 calc R . . C137 C 0.4954(3) 0.5440(4) 0.5678(2) 0.0380(16) Uani 1 1 d . . . H13A H 0.5283 0.5094 0.5859 0.046 Uiso 1 1 calc R . . H13B H 0.4670 0.5014 0.5504 0.046 Uiso 1 1 calc R . . C138 C 0.3576(3) 0.7310(4) 0.6844(2) 0.0340(15) Uani 1 1 d . . . H13C H 0.3146 0.7173 0.6729 0.041 Uiso 1 1 calc R . . H13D H 0.3677 0.7059 0.7149 0.041 Uiso 1 1 calc R . . N141 N 0.4152(2) 0.8658(3) 0.70967(16) 0.0264(11) Uani 1 1 d . . . N142 N 0.3653(2) 0.8265(3) 0.68691(17) 0.0296(12) Uani 1 1 d . . . C143 C 0.3250(3) 0.8874(5) 0.6674(2) 0.0409(17) Uani 1 1 d . . . H143 H 0.2867 0.8752 0.6495 0.049 Uiso 1 1 calc R . . C144 C 0.3493(3) 0.9711(5) 0.6779(2) 0.0381(16) Uani 1 1 d . . . H144 H 0.3319 1.0273 0.6692 0.046 Uiso 1 1 calc R . . C145 C 0.4054(3) 0.9532(4) 0.70446(19) 0.0264(13) Uani 1 1 d . . . N151 N 0.5000 0.9681(4) 0.7500 0.0230(15) Uani 1 2 d S . . C152 C 0.4522(3) 1.0119(4) 0.7275(2) 0.0283(14) Uani 1 1 d . . . C153 C 0.4505(3) 1.1041(4) 0.7278(2) 0.0344(15) Uani 1 1 d . . . H153 H 0.4158 1.1351 0.7130 0.041 Uiso 1 1 calc R . . C154 C 0.5000 1.1501(6) 0.7500 0.038(2) Uani 1 2 d S . . H154 H 0.5000 1.2132 0.7500 0.045 Uiso 1 2 calc SR . . N211 N 0.3381(2) 0.6128(3) 0.51008(17) 0.0322(12) Uani 1 1 d . . . C212 C 0.3120(3) 0.6660(5) 0.5371(2) 0.0348(16) Uani 1 1 d . . . C213 C 0.2775(3) 0.6317(5) 0.5667(2) 0.0429(17) Uani 1 1 d . . . H213 H 0.2598 0.6704 0.5856 0.051 Uiso 1 1 calc R . . C214 C 0.2686(3) 0.5407(5) 0.5686(2) 0.050(2) Uani 1 1 d . . . H214 H 0.2453 0.5162 0.5890 0.060 Uiso 1 1 calc R . . C215 C 0.2943(3) 0.4869(5) 0.5406(3) 0.0495(19) Uani 1 1 d . . . H215 H 0.2886 0.4244 0.5411 0.059 Uiso 1 1 calc R . . C216 C 0.3286(3) 0.5243(5) 0.5117(2) 0.0409(17) Uani 1 1 d . . . H216 H 0.3460 0.4865 0.4923 0.049 Uiso 1 1 calc R . . N221 N 0.3658(2) 0.7813(3) 0.50726(17) 0.0307(12) Uani 1 1 d . . . N222 N 0.3661(3) 0.8720(4) 0.50588(19) 0.0393(14) Uani 1 1 d . . . C223 C 0.3254(3) 0.9041(5) 0.5305(2) 0.0454(18) Uani 1 1 d . . . H223 H 0.3175 0.9652 0.5349 0.054 Uiso 1 1 calc R . . C224 C 0.2980(3) 0.8351(5) 0.5477(2) 0.0413(17) Uani 1 1 d . . . H224 H 0.2679 0.8374 0.5663 0.050 Uiso 1 1 calc R . . C225 C 0.3238(3) 0.7603(4) 0.5321(2) 0.0331(15) Uani 1 1 d . . . C231 C 0.4669(3) 0.9270(5) 0.5357(2) 0.0384(16) Uani 1 1 d . . . C232 C 0.5206(3) 0.8842(5) 0.5365(2) 0.0421(17) Uani 1 1 d . . . H232 H 0.5281 0.8547 0.5104 0.051 Uiso 1 1 calc R . . C233 C 0.5647(3) 0.8829(5) 0.5747(2) 0.0432(17) Uani 1 1 d . . . H233 H 0.6021 0.8530 0.5745 0.052 Uiso 1 1 calc R . . C234 C 0.5541(3) 0.9253(5) 0.6129(2) 0.0441(18) Uani 1 1 d . . . C235 C 0.5007(3) 0.9709(5) 0.6118(3) 0.052(2) Uani 1 1 d . . . H235 H 0.4934 1.0012 0.6378 0.062 Uiso 1 1 calc R . . C236 C 0.4572(3) 0.9732(5) 0.5732(2) 0.0479(19) Uani 1 1 d . . . H236 H 0.4210 1.0064 0.5726 0.057 Uiso 1 1 calc R . . C237 C 0.4173(3) 0.9216(4) 0.4949(2) 0.0430(17) Uani 1 1 d . . . H23A H 0.4042 0.9822 0.4849 0.052 Uiso 1 1 calc R . . H23B H 0.4331 0.8917 0.4702 0.052 Uiso 1 1 calc R . . C238 C 0.5993(3) 0.9203(5) 0.6559(2) 0.049(2) Uani 1 1 d . . . H23C H 0.6395 0.9400 0.6504 0.058 Uiso 1 1 calc R . . H23D H 0.5865 0.9608 0.6782 0.058 Uiso 1 1 calc R . . N241 N 0.5600(2) 0.7987(4) 0.69477(16) 0.0317(12) Uani 1 1 d . . . N242 N 0.6040(2) 0.8300(4) 0.67364(18) 0.0413(15) Uani 1 1 d . . . C243 C 0.6437(3) 0.7659(7) 0.6682(2) 0.057(2) Uani 1 1 d . . . H243 H 0.6781 0.7730 0.6540 0.068 Uiso 1 1 calc R . . C244 C 0.6269(3) 0.6904(6) 0.6859(3) 0.050(2) Uani 1 1 d . . . H244 H 0.6464 0.6342 0.6872 0.060 Uiso 1 1 calc R . . C245 C 0.5742(3) 0.7130(4) 0.7022(2) 0.0330(15) Uani 1 1 d . . . N251 N 0.5000 0.7048(5) 0.7500 0.0279(16) Uani 1 2 d S . . C252 C 0.5364(3) 0.6598(4) 0.7271(2) 0.0372(16) Uani 1 1 d . . . C253 C 0.5381(3) 0.5676(5) 0.7269(3) 0.049(2) Uani 1 1 d . . . H253 H 0.5650 0.5368 0.7113 0.059 Uiso 1 1 calc R . . C254 C 0.5000 0.5215(7) 0.7500 0.054(3) Uani 1 2 d S . . H254 H 0.5000 0.4584 0.7500 0.064 Uiso 1 2 calc SR . . O11 O 0.37982(19) 0.5758(3) 0.42810(14) 0.0347(10) Uani 1 1 d . . . C13 C 0.3373(3) 0.5932(5) 0.3957(2) 0.0336(15) Uani 1 1 d . . . O12 O 0.30444(18) 0.6597(3) 0.39485(15) 0.0357(11) Uani 1 1 d . . . C14 C 0.3304(3) 0.5292(5) 0.3564(2) 0.050(2) Uani 1 1 d . . . H14A H 0.3102 0.4750 0.3639 0.076 Uiso 1 1 calc R . . H14B H 0.3706 0.5143 0.3498 0.076 Uiso 1 1 calc R . . H14C H 0.3061 0.5572 0.3302 0.076 Uiso 1 1 calc R . . C21 C 0.6902(7) 0.3188(9) 0.7910(5) 0.137(5) Uiso 1 1 d D . . H21A H 0.6994 0.2572 0.7969 0.205 Uiso 0.69(19) 1 d PR A 1 H21B H 0.7221 0.3459 0.7784 0.205 Uiso 0.69(19) 1 d PR A 1 H21C H 0.6864 0.3482 0.8184 0.205 Uiso 0.69(19) 1 d PR A 1 H21D H 0.7180 0.3340 0.8176 0.205 Uiso 0.31(19) 1 d PR A 2 H21E H 0.6965 0.2581 0.7832 0.205 Uiso 0.31(19) 1 d PR A 2 H21F H 0.6968 0.3569 0.7670 0.205 Uiso 0.31(19) 1 d PR A 2 C22 C 0.6304(11) 0.3275(18) 0.7581(9) 0.088(5) Uiso 0.409(11) 1 d PDU B 1 C22' C 0.6262(8) 0.3304(12) 0.7999(7) 0.086(5) Uiso 0.591(11) 1 d PDU B 2 N23 N 0.5872(12) 0.342(2) 0.7338(10) 0.148(12) Uiso 0.409(11) 1 d PD B 1 N23' N 0.5767(7) 0.3352(10) 0.8000(6) 0.096(5) Uiso 0.591(11) 1 d PD B 2 P1 P 0.28406(10) 0.16505(18) 0.57823(9) 0.0668(7) Uani 1 1 d D . . F11 F 0.3363(5) 0.1707(10) 0.6212(4) 0.077(3) Uiso 0.553(19) 1 d PDU C 1 F11' F 0.3441(5) 0.1376(11) 0.6109(5) 0.069(3) Uiso 0.447(19) 1 d PDU C 2 F12 F 0.2503(5) 0.1719(9) 0.6206(4) 0.085(3) Uiso 0.553(19) 1 d PDU C 1 F12' F 0.2368(7) 0.2040(12) 0.6029(7) 0.101(4) Uiso 0.447(19) 1 d PDU C 2 F13 F 0.2688(3) 0.0609(4) 0.5821(2) 0.103(2) Uani 1 1 d . C . F14 F 0.2289(3) 0.1717(4) 0.5398(2) 0.112(2) Uani 1 1 d . C . F15 F 0.3268(3) 0.1325(5) 0.5428(3) 0.126(2) Uani 1 1 d . C . F16 F 0.3057(3) 0.2592(3) 0.5691(2) 0.103(2) Uani 1 1 d . C . P2 P 0.27493(9) 0.92183(15) 0.28004(7) 0.0487(5) Uani 1 1 d . . . F21 F 0.2850(3) 0.9366(5) 0.33185(17) 0.108(2) Uani 1 1 d . . . F22 F 0.2652(2) 0.8187(3) 0.2877(2) 0.0864(18) Uani 1 1 d . . . F23 F 0.2044(2) 0.9384(4) 0.2761(2) 0.0867(18) Uani 1 1 d . . . F24 F 0.2647(2) 0.9056(4) 0.22779(16) 0.0808(16) Uani 1 1 d . . . F25 F 0.2860(2) 1.0234(3) 0.27280(17) 0.0676(14) Uani 1 1 d . . . F26 F 0.34536(19) 0.9056(3) 0.28274(17) 0.0718(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0224(5) 0.0281(6) 0.0258(6) 0.000 0.0019(4) 0.000 Cu2 0.0251(4) 0.0335(4) 0.0290(4) 0.0006(3) 0.0065(3) 0.0010(3) N111 0.030(3) 0.039(3) 0.027(3) -0.001(2) -0.001(2) 0.001(2) C112 0.030(3) 0.032(4) 0.031(4) -0.003(3) 0.002(3) 0.001(3) C113 0.033(4) 0.069(5) 0.042(4) 0.013(4) 0.013(3) -0.005(4) C114 0.056(5) 0.092(7) 0.050(5) 0.030(5) 0.022(4) -0.002(5) C115 0.053(5) 0.074(6) 0.050(5) 0.025(4) 0.001(4) -0.010(4) C116 0.030(4) 0.042(4) 0.041(4) 0.003(3) 0.000(3) -0.003(3) N121 0.023(3) 0.032(3) 0.028(3) 0.000(2) 0.003(2) 0.006(2) N122 0.032(3) 0.032(3) 0.028(3) 0.004(2) 0.008(2) 0.008(2) C123 0.029(4) 0.042(4) 0.033(4) 0.001(3) 0.004(3) 0.004(3) C124 0.023(3) 0.041(4) 0.036(4) 0.004(3) 0.003(3) 0.004(3) C125 0.030(3) 0.032(4) 0.032(4) -0.002(3) 0.007(3) -0.001(3) C131 0.030(3) 0.037(4) 0.021(3) -0.002(3) 0.001(3) 0.006(3) C132 0.047(4) 0.030(4) 0.036(4) 0.002(3) 0.009(3) 0.001(3) C133 0.037(4) 0.048(4) 0.029(4) 0.004(3) 0.011(3) -0.008(3) C134 0.021(3) 0.038(4) 0.027(3) -0.006(3) 0.003(3) -0.003(3) C135 0.028(3) 0.027(3) 0.027(3) -0.001(3) 0.003(3) -0.002(3) C136 0.028(3) 0.033(4) 0.026(3) 0.001(3) 0.008(3) 0.000(3) C137 0.045(4) 0.040(4) 0.029(4) 0.003(3) 0.009(3) 0.007(3) C138 0.029(3) 0.042(4) 0.032(4) -0.009(3) 0.006(3) -0.010(3) N141 0.021(3) 0.035(3) 0.022(3) -0.006(2) 0.001(2) -0.001(2) N142 0.018(2) 0.043(3) 0.027(3) -0.008(2) 0.002(2) 0.000(2) C143 0.031(4) 0.059(5) 0.030(4) -0.005(3) -0.002(3) 0.014(3) C144 0.031(4) 0.044(4) 0.040(4) 0.002(3) 0.007(3) 0.012(3) C145 0.024(3) 0.037(4) 0.019(3) -0.001(3) 0.007(3) 0.007(3) N151 0.018(3) 0.030(4) 0.020(4) 0.000 0.002(3) 0.000 C152 0.027(3) 0.031(4) 0.029(3) 0.000(3) 0.012(3) 0.004(3) C153 0.039(4) 0.035(4) 0.031(4) 0.005(3) 0.012(3) 0.008(3) C154 0.053(6) 0.030(5) 0.037(6) 0.000 0.027(5) 0.000 N211 0.027(3) 0.034(3) 0.035(3) -0.002(2) 0.005(2) 0.003(2) C212 0.021(3) 0.058(5) 0.024(3) -0.001(3) -0.002(3) 0.002(3) C213 0.030(4) 0.065(5) 0.034(4) -0.002(4) 0.007(3) -0.003(3) C214 0.037(4) 0.070(6) 0.042(4) 0.008(4) 0.009(4) -0.015(4) C215 0.047(4) 0.051(5) 0.051(5) 0.008(4) 0.010(4) -0.009(4) C216 0.040(4) 0.042(4) 0.044(4) 0.003(3) 0.017(3) 0.004(3) N221 0.028(3) 0.033(3) 0.030(3) 0.004(2) 0.000(2) 0.005(2) N222 0.042(3) 0.031(3) 0.043(3) -0.001(3) 0.000(3) -0.001(3) C223 0.040(4) 0.045(4) 0.048(5) -0.015(4) -0.001(4) 0.012(3) C224 0.026(3) 0.062(5) 0.035(4) -0.014(4) 0.000(3) 0.004(3) C225 0.022(3) 0.043(4) 0.032(4) -0.005(3) -0.004(3) 0.001(3) C231 0.048(4) 0.041(4) 0.026(4) 0.001(3) 0.004(3) -0.010(3) C232 0.058(5) 0.035(4) 0.032(4) -0.002(3) 0.006(4) -0.005(3) C233 0.052(4) 0.038(4) 0.041(4) 0.002(3) 0.011(4) -0.007(3) C234 0.047(4) 0.054(5) 0.032(4) -0.003(3) 0.009(3) -0.025(4) C235 0.049(5) 0.068(5) 0.041(4) -0.011(4) 0.015(4) -0.024(4) C236 0.043(4) 0.059(5) 0.041(4) -0.010(4) 0.008(4) -0.012(4) C237 0.054(5) 0.031(4) 0.043(4) 0.001(3) 0.003(4) -0.010(3) C238 0.038(4) 0.074(6) 0.034(4) 0.000(4) 0.006(3) -0.025(4) N241 0.030(3) 0.045(3) 0.020(3) -0.006(2) 0.003(2) -0.006(2) N242 0.028(3) 0.070(4) 0.026(3) -0.003(3) 0.002(2) -0.012(3) C243 0.034(4) 0.101(7) 0.036(4) -0.004(5) 0.008(4) 0.013(4) C244 0.040(4) 0.066(5) 0.043(5) -0.013(4) 0.005(4) 0.023(4) C245 0.034(4) 0.044(4) 0.020(3) -0.010(3) 0.000(3) 0.010(3) N251 0.023(4) 0.034(4) 0.026(4) 0.000 0.001(3) 0.000 C252 0.031(3) 0.034(4) 0.041(4) -0.004(3) -0.012(3) 0.002(3) C253 0.051(5) 0.040(4) 0.052(5) -0.011(4) -0.007(4) 0.009(4) C254 0.060(7) 0.021(5) 0.070(8) 0.000 -0.017(6) 0.000 O11 0.029(2) 0.042(3) 0.032(3) -0.002(2) 0.004(2) 0.001(2) C13 0.024(3) 0.045(4) 0.032(4) -0.001(3) 0.006(3) -0.004(3) O12 0.024(2) 0.040(3) 0.043(3) 0.001(2) 0.005(2) 0.002(2) C14 0.047(4) 0.057(5) 0.045(5) -0.016(4) 0.002(4) 0.011(4) P1 0.0412(12) 0.0862(19) 0.0711(16) 0.0255(14) 0.0044(11) -0.0130(12) F13 0.119(5) 0.074(4) 0.119(5) 0.003(4) 0.028(4) -0.005(4) F14 0.066(4) 0.115(5) 0.137(6) 0.019(4) -0.038(4) 0.001(3) F15 0.098(5) 0.134(6) 0.157(7) -0.012(5) 0.052(5) 0.001(4) F16 0.090(4) 0.047(3) 0.162(6) 0.028(4) -0.005(4) -0.009(3) P2 0.0389(11) 0.0598(14) 0.0503(13) 0.0006(10) 0.0156(9) -0.0131(10) F21 0.116(5) 0.172(6) 0.042(3) -0.003(3) 0.031(3) -0.041(4) F22 0.076(4) 0.059(3) 0.137(5) 0.013(3) 0.055(4) -0.008(3) F23 0.041(3) 0.085(4) 0.138(5) 0.006(4) 0.027(3) -0.008(3) F24 0.080(4) 0.109(4) 0.050(3) -0.009(3) 0.002(3) -0.035(3) F25 0.060(3) 0.055(3) 0.090(4) -0.003(3) 0.020(3) -0.017(2) F26 0.036(2) 0.096(4) 0.086(4) 0.013(3) 0.017(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. ; 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 Cu1 N151 1.978(7) . ? Cu1 N251 1.987(7) . ? Cu1 N141 2.123(5) 2_656 ? Cu1 N141 2.123(5) . ? Cu1 N241 2.394(5) . ? Cu1 N241 2.394(5) 2_656 ? Cu2 O11 1.958(4) . ? Cu2 N211 2.002(5) . ? Cu2 N111 2.011(5) . ? Cu2 N221 2.068(5) . ? Cu2 N121 2.282(5) . ? N111 C116 1.355(8) . ? N111 C112 1.360(8) . ? C112 C113 1.367(9) . ? C112 C125 1.464(9) . ? C113 C114 1.364(10) . ? C114 C115 1.396(11) . ? C115 C116 1.365(10) . ? N121 C125 1.336(8) . ? N121 N122 1.349(7) . ? N122 C123 1.352(8) . ? N122 C137 1.455(8) . ? C123 C124 1.351(9) . ? C124 C125 1.400(9) . ? C131 C132 1.386(9) . ? C131 C136 1.398(8) . ? C131 C137 1.516(8) . ? C132 C133 1.390(9) . ? C133 C134 1.384(9) . ? C134 C135 1.369(8) . ? C134 C138 1.516(8) . ? C135 C136 1.373(8) . ? C138 N142 1.450(8) . ? N141 C145 1.339(8) . ? N141 N142 1.347(6) . ? N142 C143 1.351(8) . ? C143 C144 1.389(10) . ? C144 C145 1.399(8) . ? C145 C152 1.457(8) . ? N151 C152 1.341(7) 2_656 ? N151 C152 1.341(7) . ? C152 C153 1.389(9) . ? C153 C154 1.381(8) . ? C154 C153 1.381(8) 2_656 ? N211 C212 1.351(8) . ? N211 C216 1.351(8) . ? C212 C213 1.383(9) . ? C212 C225 1.458(9) . ? C213 C214 1.388(10) . ? C214 C215 1.372(11) . ? C215 C216 1.382(9) . ? N221 C225 1.341(8) . ? N221 N222 1.368(7) . ? N222 C223 1.364(9) . ? N222 C237 1.454(8) . ? C223 C224 1.358(10) . ? C224 C225 1.386(9) . ? C231 C232 1.362(10) . ? C231 C236 1.385(9) . ? C231 C237 1.519(9) . ? C232 C233 1.390(10) . ? C233 C234 1.383(10) . ? C234 C235 1.374(11) . ? C234 C238 1.513(10) . ? C235 C236 1.391(10) . ? C238 N242 1.460(9) . ? N241 C245 1.339(8) . ? N241 N242 1.349(7) . ? N242 C243 1.342(9) . ? C243 C244 1.341(11) . ? C244 C245 1.400(9) . ? C245 C252 1.465(9) . ? N251 C252 1.344(8) . ? N251 C252 1.344(8) 2_656 ? C252 C253 1.389(9) . ? C253 C254 1.381(9) . ? C254 C253 1.381(9) 2_656 ? O11 C13 1.276(7) . ? C13 O12 1.240(7) . ? C13 C14 1.521(9) . ? C21 C22' 1.514(18) . ? C21 C22 1.53(2) . ? C22 N23 1.13(2) . ? C22' N23' 1.112(18) . ? P1 F12' 1.516(11) . ? P1 F16 1.539(5) . ? P1 F14 1.552(6) . ? P1 F11' 1.584(10) . ? P1 F11 1.600(9) . ? P1 F12 1.606(9) . ? P1 F13 1.615(6) . ? P1 F15 1.634(7) . ? P2 F21 1.569(5) . ? P2 F25 1.571(5) . ? P2 F23 1.583(5) . ? P2 F26 1.584(5) . ? P2 F24 1.585(5) . ? P2 F22 1.591(5) . ? 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 N151 Cu1 N251 180.000(4) . . ? N151 Cu1 N141 78.12(14) . 2_656 ? N251 Cu1 N141 101.88(14) . 2_656 ? N151 Cu1 N141 78.12(14) . . ? N251 Cu1 N141 101.88(14) . . ? N141 Cu1 N141 156.2(3) 2_656 . ? N151 Cu1 N241 103.88(14) . . ? N251 Cu1 N241 76.12(13) . . ? N141 Cu1 N241 84.28(18) 2_656 . ? N141 Cu1 N241 101.45(18) . . ? N151 Cu1 N241 103.88(13) . 2_656 ? N251 Cu1 N241 76.12(13) . 2_656 ? N141 Cu1 N241 101.45(18) 2_656 2_656 ? N141 Cu1 N241 84.28(18) . 2_656 ? N241 Cu1 N241 152.2(3) . 2_656 ? O11 Cu2 N211 92.6(2) . . ? O11 Cu2 N111 88.2(2) . . ? N211 Cu2 N111 178.2(2) . . ? O11 Cu2 N221 160.05(19) . . ? N211 Cu2 N221 80.0(2) . . ? N111 Cu2 N221 98.8(2) . . ? O11 Cu2 N121 93.57(18) . . ? N211 Cu2 N121 103.72(19) . . ? N111 Cu2 N121 77.83(19) . . ? N221 Cu2 N121 106.15(19) . . ? C116 N111 C112 117.0(6) . . ? C116 N111 Cu2 124.0(4) . . ? C112 N111 Cu2 118.1(4) . . ? N111 C112 C113 122.2(6) . . ? N111 C112 C125 115.7(5) . . ? C113 C112 C125 122.2(6) . . ? C114 C113 C112 119.6(7) . . ? C113 C114 C115 120.0(7) . . ? C116 C115 C114 117.3(7) . . ? N111 C116 C115 124.0(7) . . ? C125 N121 N122 104.7(5) . . ? C125 N121 Cu2 108.5(4) . . ? N122 N121 Cu2 145.2(4) . . ? N121 N122 C123 111.0(5) . . ? N121 N122 C137 120.3(5) . . ? C123 N122 C137 128.7(5) . . ? C124 C123 N122 108.4(6) . . ? C123 C124 C125 104.4(6) . . ? N121 C125 C124 111.5(6) . . ? N121 C125 C112 118.3(5) . . ? C124 C125 C112 130.2(6) . . ? C132 C131 C136 119.3(6) . . ? C132 C131 C137 118.2(6) . . ? C136 C131 C137 122.5(6) . . ? C131 C132 C133 119.6(6) . . ? C134 C133 C132 120.8(6) . . ? C135 C134 C133 118.9(6) . . ? C135 C134 C138 123.2(6) . . ? C133 C134 C138 117.8(6) . . ? C134 C135 C136 121.5(6) . . ? C135 C136 C131 119.8(6) . . ? N122 C137 C131 113.3(5) . . ? N142 C138 C134 113.6(5) . . ? C145 N141 N142 105.5(5) . . ? C145 N141 Cu1 112.5(4) . . ? N142 N141 Cu1 142.0(4) . . ? N141 N142 C143 111.2(5) . . ? N141 N142 C138 122.9(5) . . ? C143 N142 C138 125.9(5) . . ? N142 C143 C144 108.0(6) . . ? C143 C144 C145 103.7(6) . . ? N141 C145 C144 111.7(6) . . ? N141 C145 C152 116.8(5) . . ? C144 C145 C152 131.5(6) . . ? C152 N151 C152 121.0(7) 2_656 . ? C152 N151 Cu1 119.5(4) 2_656 . ? C152 N151 Cu1 119.5(4) . . ? N151 C152 C153 120.6(6) . . ? N151 C152 C145 113.1(5) . . ? C153 C152 C145 126.3(6) . . ? C154 C153 C152 118.9(7) . . ? C153 C154 C153 119.8(9) . 2_656 ? C212 N211 C216 118.4(6) . . ? C212 N211 Cu2 115.8(4) . . ? C216 N211 Cu2 125.8(4) . . ? N211 C212 C213 121.6(7) . . ? N211 C212 C225 114.2(6) . . ? C213 C212 C225 124.3(6) . . ? C212 C213 C214 119.7(7) . . ? C215 C214 C213 118.6(7) . . ? C214 C215 C216 119.5(7) . . ? N211 C216 C215 122.2(7) . . ? C225 N221 N222 105.1(5) . . ? C225 N221 Cu2 112.2(4) . . ? N222 N221 Cu2 139.5(4) . . ? C223 N222 N221 109.3(6) . . ? C223 N222 C237 124.9(6) . . ? N221 N222 C237 121.9(5) . . ? C224 C223 N222 109.2(6) . . ? C223 C224 C225 104.3(6) . . ? N221 C225 C224 112.1(6) . . ? N221 C225 C212 116.4(6) . . ? C224 C225 C212 131.4(6) . . ? C232 C231 C236 119.0(7) . . ? C232 C231 C237 120.6(6) . . ? C236 C231 C237 120.3(7) . . ? C231 C232 C233 121.4(7) . . ? C234 C233 C232 119.7(7) . . ? C235 C234 C233 119.0(7) . . ? C235 C234 C238 119.7(7) . . ? C233 C234 C238 121.2(7) . . ? C234 C235 C236 120.9(7) . . ? C231 C236 C235 119.8(7) . . ? N222 C237 C231 109.5(6) . . ? N242 C238 C234 111.2(6) . . ? C245 N241 N242 104.3(5) . . ? C245 N241 Cu1 104.9(4) . . ? N242 N241 Cu1 142.5(4) . . ? C243 N242 N241 111.2(6) . . ? C243 N242 C238 129.1(6) . . ? N241 N242 C238 119.3(6) . . ? C244 C243 N242 108.8(7) . . ? C243 C244 C245 104.4(7) . . ? N241 C245 C244 111.4(6) . . ? N241 C245 C252 118.3(5) . . ? C244 C245 C252 130.3(7) . . ? C252 N251 C252 119.4(8) . 2_656 ? C252 N251 Cu1 120.3(4) . . ? C252 N251 Cu1 120.3(4) 2_656 . ? N251 C252 C253 121.6(7) . . ? N251 C252 C245 116.6(6) . . ? C253 C252 C245 121.8(7) . . ? C254 C253 C252 118.8(8) . . ? C253 C254 C253 119.7(10) . 2_656 ? C13 O11 Cu2 109.5(4) . . ? O12 C13 O11 122.9(6) . . ? O12 C13 C14 121.0(6) . . ? O11 C13 C14 116.0(6) . . ? C22' C21 C22 50.2(12) . . ? N23 C22 C21 174(3) . . ? N23' C22' C21 169(2) . . ? F12' P1 F16 90.1(8) . . ? F12' P1 F14 79.3(8) . . ? F16 P1 F14 92.3(4) . . ? F12' P1 F11' 112.3(12) . . ? F16 P1 F11' 95.4(6) . . ? F14 P1 F11' 166.0(8) . . ? F12' P1 F11 92.9(11) . . ? F16 P1 F11 83.6(5) . . ? F14 P1 F11 171.2(7) . . ? F11' P1 F11 22.7(5) . . ? F12' P1 F12 27.6(7) . . ? F16 P1 F12 107.0(6) . . ? F14 P1 F12 100.2(6) . . ? F11' P1 F12 88.8(9) . . ? F11 P1 F12 73.7(8) . . ? F12' P1 F13 99.5(8) . . ? F16 P1 F13 170.3(4) . . ? F14 P1 F13 88.1(4) . . ? F11' P1 F13 82.5(6) . . ? F11 P1 F13 97.3(5) . . ? F12 P1 F13 82.4(5) . . ? F12' P1 F15 168.4(9) . . ? F16 P1 F15 85.3(4) . . ? F14 P1 F15 90.2(4) . . ? F11' P1 F15 78.8(7) . . ? F11 P1 F15 97.2(6) . . ? F12 P1 F15 163.3(7) . . ? F13 P1 F15 85.0(4) . . ? F21 P2 F25 90.2(3) . . ? F21 P2 F23 91.3(3) . . ? F25 P2 F23 90.9(3) . . ? F21 P2 F26 90.0(3) . . ? F25 P2 F26 88.7(3) . . ? F23 P2 F26 178.6(3) . . ? F21 P2 F24 179.3(4) . . ? F25 P2 F24 90.5(3) . . ? F23 P2 F24 88.7(3) . . ? F26 P2 F24 90.0(3) . . ? F21 P2 F22 89.5(4) . . ? F25 P2 F22 178.8(3) . . ? F23 P2 F22 90.3(3) . . ? F26 P2 F22 90.1(3) . . ? F24 P2 F22 89.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Cu2 N111 C116 77.5(5) . . . . ? N211 Cu2 N111 C116 -37(7) . . . . ? N221 Cu2 N111 C116 -83.7(5) . . . . ? N121 Cu2 N111 C116 171.6(6) . . . . ? O11 Cu2 N111 C112 -91.5(5) . . . . ? N211 Cu2 N111 C112 154(7) . . . . ? N221 Cu2 N111 C112 107.3(5) . . . . ? N121 Cu2 N111 C112 2.6(4) . . . . ? C116 N111 C112 C113 0.5(10) . . . . ? Cu2 N111 C112 C113 170.3(5) . . . . ? C116 N111 C112 C125 -179.4(6) . . . . ? Cu2 N111 C112 C125 -9.6(7) . . . . ? N111 C112 C113 C114 -1.7(12) . . . . ? C125 C112 C113 C114 178.2(7) . . . . ? C112 C113 C114 C115 1.6(14) . . . . ? C113 C114 C115 C116 -0.3(14) . . . . ? C112 N111 C116 C115 0.9(10) . . . . ? Cu2 N111 C116 C115 -168.3(6) . . . . ? C114 C115 C116 N111 -0.9(12) . . . . ? O11 Cu2 N121 C125 92.5(4) . . . . ? N211 Cu2 N121 C125 -174.0(4) . . . . ? N111 Cu2 N121 C125 5.1(4) . . . . ? N221 Cu2 N121 C125 -90.6(4) . . . . ? O11 Cu2 N121 N122 -105.5(7) . . . . ? N211 Cu2 N121 N122 -12.0(7) . . . . ? N111 Cu2 N121 N122 167.2(7) . . . . ? N221 Cu2 N121 N122 71.4(7) . . . . ? C125 N121 N122 C123 2.4(7) . . . . ? Cu2 N121 N122 C123 -160.0(6) . . . . ? C125 N121 N122 C137 -178.5(5) . . . . ? Cu2 N121 N122 C137 19.0(10) . . . . ? N121 N122 C123 C124 -1.8(7) . . . . ? C137 N122 C123 C124 179.2(6) . . . . ? N122 C123 C124 C125 0.4(7) . . . . ? N122 N121 C125 C124 -2.1(7) . . . . ? Cu2 N121 C125 C124 167.4(4) . . . . ? N122 N121 C125 C112 178.7(5) . . . . ? Cu2 N121 C125 C112 -11.8(7) . . . . ? C123 C124 C125 N121 1.1(7) . . . . ? C123 C124 C125 C112 -179.9(6) . . . . ? N111 C112 C125 N121 14.8(8) . . . . ? C113 C112 C125 N121 -165.0(6) . . . . ? N111 C112 C125 C124 -164.2(6) . . . . ? C113 C112 C125 C124 16.0(11) . . . . ? C136 C131 C132 C133 1.3(10) . . . . ? C137 C131 C132 C133 -178.6(6) . . . . ? C131 C132 C133 C134 0.8(10) . . . . ? C132 C133 C134 C135 -2.5(10) . . . . ? C132 C133 C134 C138 176.6(6) . . . . ? C133 C134 C135 C136 2.0(9) . . . . ? C138 C134 C135 C136 -177.0(6) . . . . ? C134 C135 C136 C131 0.1(9) . . . . ? C132 C131 C136 C135 -1.8(9) . . . . ? C137 C131 C136 C135 178.2(6) . . . . ? N121 N122 C137 C131 -75.5(7) . . . . ? C123 N122 C137 C131 103.4(7) . . . . ? C132 C131 C137 N122 172.4(6) . . . . ? C136 C131 C137 N122 -7.6(9) . . . . ? C135 C134 C138 N142 -7.3(9) . . . . ? C133 C134 C138 N142 173.6(5) . . . . ? N151 Cu1 N141 C145 0.7(4) . . . . ? N251 Cu1 N141 C145 -179.3(4) . . . . ? N141 Cu1 N141 C145 0.7(4) 2_656 . . . ? N241 Cu1 N141 C145 -101.2(4) . . . . ? N241 Cu1 N141 C145 106.2(4) 2_656 . . . ? N151 Cu1 N141 N142 -178.2(6) . . . . ? N251 Cu1 N141 N142 1.8(6) . . . . ? N141 Cu1 N141 N142 -178.2(6) 2_656 . . . ? N241 Cu1 N141 N142 79.8(6) . . . . ? N241 Cu1 N141 N142 -72.7(6) 2_656 . . . ? C145 N141 N142 C143 0.5(6) . . . . ? Cu1 N141 N142 C143 179.5(5) . . . . ? C145 N141 N142 C138 -179.7(5) . . . . ? Cu1 N141 N142 C138 -0.7(9) . . . . ? C134 C138 N142 N141 -72.8(7) . . . . ? C134 C138 N142 C143 107.0(7) . . . . ? N141 N142 C143 C144 -0.3(7) . . . . ? C138 N142 C143 C144 179.8(6) . . . . ? N142 C143 C144 C145 0.0(7) . . . . ? N142 N141 C145 C144 -0.5(7) . . . . ? Cu1 N141 C145 C144 -179.8(4) . . . . ? N142 N141 C145 C152 177.7(5) . . . . ? Cu1 N141 C145 C152 -1.6(6) . . . . ? C143 C144 C145 N141 0.3(7) . . . . ? C143 C144 C145 C152 -177.6(6) . . . . ? N251 Cu1 N151 C152 -35(100) . . . 2_656 ? N141 Cu1 N151 C152 0.3(3) 2_656 . . 2_656 ? N141 Cu1 N151 C152 -179.7(3) . . . 2_656 ? N241 Cu1 N151 C152 -80.7(3) . . . 2_656 ? N241 Cu1 N151 C152 99.3(3) 2_656 . . 2_656 ? N251 Cu1 N151 C152 145(100) . . . . ? N141 Cu1 N151 C152 -179.7(3) 2_656 . . . ? N141 Cu1 N151 C152 0.3(3) . . . . ? N241 Cu1 N151 C152 99.3(3) . . . . ? N241 Cu1 N151 C152 -80.7(3) 2_656 . . . ? C152 N151 C152 C153 -1.5(4) 2_656 . . . ? Cu1 N151 C152 C153 178.5(4) . . . . ? C152 N151 C152 C145 178.8(5) 2_656 . . . ? Cu1 N151 C152 C145 -1.2(5) . . . . ? N141 C145 C152 N151 1.8(7) . . . . ? C144 C145 C152 N151 179.6(6) . . . . ? N141 C145 C152 C153 -177.8(6) . . . . ? C144 C145 C152 C153 0.0(10) . . . . ? N151 C152 C153 C154 3.0(8) . . . . ? C145 C152 C153 C154 -177.4(5) . . . . ? C152 C153 C154 C153 -1.4(4) . . . 2_656 ? O11 Cu2 N211 C212 -157.3(4) . . . . ? N111 Cu2 N211 C212 -43(7) . . . . ? N221 Cu2 N211 C212 4.1(4) . . . . ? N121 Cu2 N211 C212 108.4(4) . . . . ? O11 Cu2 N211 C216 22.9(5) . . . . ? N111 Cu2 N211 C216 137(7) . . . . ? N221 Cu2 N211 C216 -175.7(6) . . . . ? N121 Cu2 N211 C216 -71.4(5) . . . . ? C216 N211 C212 C213 1.5(9) . . . . ? Cu2 N211 C212 C213 -178.3(5) . . . . ? C216 N211 C212 C225 -178.6(5) . . . . ? Cu2 N211 C212 C225 1.6(7) . . . . ? N211 C212 C213 C214 -0.6(10) . . . . ? C225 C212 C213 C214 179.5(6) . . . . ? C212 C213 C214 C215 -0.6(11) . . . . ? C213 C214 C215 C216 0.7(11) . . . . ? C212 N211 C216 C215 -1.4(10) . . . . ? Cu2 N211 C216 C215 178.4(5) . . . . ? C214 C215 C216 N211 0.3(11) . . . . ? O11 Cu2 N221 C225 60.0(8) . . . . ? N211 Cu2 N221 C225 -9.5(4) . . . . ? N111 Cu2 N221 C225 169.2(4) . . . . ? N121 Cu2 N221 C225 -111.0(4) . . . . ? O11 Cu2 N221 N222 -95.5(8) . . . . ? N211 Cu2 N221 N222 -164.9(6) . . . . ? N111 Cu2 N221 N222 13.8(6) . . . . ? N121 Cu2 N221 N222 93.5(6) . . . . ? C225 N221 N222 C223 1.2(7) . . . . ? Cu2 N221 N222 C223 157.8(5) . . . . ? C225 N221 N222 C237 159.8(6) . . . . ? Cu2 N221 N222 C237 -43.6(9) . . . . ? N221 N222 C223 C224 -0.6(8) . . . . ? C237 N222 C223 C224 -158.4(6) . . . . ? N222 C223 C224 C225 -0.3(8) . . . . ? N222 N221 C225 C224 -1.5(7) . . . . ? Cu2 N221 C225 C224 -165.3(4) . . . . ? N222 N221 C225 C212 177.0(5) . . . . ? Cu2 N221 C225 C212 13.2(7) . . . . ? C223 C224 C225 N221 1.2(8) . . . . ? C223 C224 C225 C212 -177.1(7) . . . . ? N211 C212 C225 N221 -10.2(8) . . . . ? C213 C212 C225 N221 169.7(6) . . . . ? N211 C212 C225 C224 168.0(6) . . . . ? C213 C212 C225 C224 -12.1(11) . . . . ? C236 C231 C232 C233 2.8(10) . . . . ? C237 C231 C232 C233 -175.2(6) . . . . ? C231 C232 C233 C234 0.4(10) . . . . ? C232 C233 C234 C235 -2.4(10) . . . . ? C232 C233 C234 C238 175.9(6) . . . . ? C233 C234 C235 C236 1.3(11) . . . . ? C238 C234 C235 C236 -177.1(6) . . . . ? C232 C231 C236 C235 -3.9(10) . . . . ? C237 C231 C236 C235 174.1(6) . . . . ? C234 C235 C236 C231 1.9(11) . . . . ? C223 N222 C237 C231 75.4(8) . . . . ? N221 N222 C237 C231 -79.8(7) . . . . ? C232 C231 C237 N222 112.7(7) . . . . ? C236 C231 C237 N222 -65.3(8) . . . . ? C235 C234 C238 N242 111.9(8) . . . . ? C233 C234 C238 N242 -66.4(8) . . . . ? N151 Cu1 N241 C245 164.1(4) . . . . ? N251 Cu1 N241 C245 -15.9(4) . . . . ? N141 Cu1 N241 C245 87.8(4) 2_656 . . . ? N141 Cu1 N241 C245 -115.5(4) . . . . ? N241 Cu1 N241 C245 -15.9(4) 2_656 . . . ? N151 Cu1 N241 N242 24.1(7) . . . . ? N251 Cu1 N241 N242 -155.9(7) . . . . ? N141 Cu1 N241 N242 -52.2(7) 2_656 . . . ? N141 Cu1 N241 N242 104.5(7) . . . . ? N241 Cu1 N241 N242 -155.9(7) 2_656 . . . ? C245 N241 N242 C243 0.1(7) . . . . ? Cu1 N241 N242 C243 140.3(6) . . . . ? C245 N241 N242 C238 173.4(5) . . . . ? Cu1 N241 N242 C238 -46.4(9) . . . . ? C234 C238 N242 C243 94.8(8) . . . . ? C234 C238 N242 N241 -77.1(7) . . . . ? N241 N242 C243 C244 -0.3(8) . . . . ? C238 N242 C243 C244 -172.8(6) . . . . ? N242 C243 C244 C245 0.4(8) . . . . ? N242 N241 C245 C244 0.1(7) . . . . ? Cu1 N241 C245 C244 -156.1(5) . . . . ? N242 N241 C245 C252 177.0(5) . . . . ? Cu1 N241 C245 C252 20.8(6) . . . . ? C243 C244 C245 N241 -0.3(8) . . . . ? C243 C244 C245 C252 -176.7(7) . . . . ? N151 Cu1 N251 C252 -36(100) . . . . ? N141 Cu1 N251 C252 -71.9(3) 2_656 . . . ? N141 Cu1 N251 C252 108.1(3) . . . . ? N241 Cu1 N251 C252 9.1(3) . . . . ? N241 Cu1 N251 C252 -170.9(3) 2_656 . . . ? N151 Cu1 N251 C252 144(100) . . . 2_656 ? N141 Cu1 N251 C252 108.1(3) 2_656 . . 2_656 ? N141 Cu1 N251 C252 -71.9(3) . . . 2_656 ? N241 Cu1 N251 C252 -170.9(3) . . . 2_656 ? N241 Cu1 N251 C252 9.1(3) 2_656 . . 2_656 ? C252 N251 C252 C253 -0.9(5) 2_656 . . . ? Cu1 N251 C252 C253 179.1(5) . . . . ? C252 N251 C252 C245 179.0(6) 2_656 . . . ? Cu1 N251 C252 C245 -1.0(6) . . . . ? N241 C245 C252 N251 -16.0(8) . . . . ? C244 C245 C252 N251 160.1(6) . . . . ? N241 C245 C252 C253 163.9(6) . . . . ? C244 C245 C252 C253 -19.9(11) . . . . ? N251 C252 C253 C254 1.9(9) . . . . ? C245 C252 C253 C254 -178.1(5) . . . . ? C252 C253 C254 C253 -0.9(4) . . . 2_656 ? N211 Cu2 O11 C13 97.3(4) . . . . ? N111 Cu2 O11 C13 -81.1(4) . . . . ? N221 Cu2 O11 C13 29.9(8) . . . . ? N121 Cu2 O11 C13 -158.8(4) . . . . ? Cu2 O11 C13 O12 -5.6(7) . . . . ? Cu2 O11 C13 C14 171.9(5) . . . . ? C22' C21 C22 N23 92(30) . . . . ? C22 C21 C22' N23' 16(11) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.472 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.128 #===END data_agfeag _database_code_depnum_ccdc_archive 'CCDC 265434' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H70 Ag2 B4 F16 Fe N22' _chemical_formula_weight 2030.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.6701(18) _cell_length_b 13.7810(8) _cell_length_c 21.3348(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.511(2) _cell_angle_gamma 90.00 _cell_volume 8940.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.075 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4096 _exptl_absorpt_coefficient_mu 5.553 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.67 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PROTEUM' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20405 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 70.43 _reflns_number_total 7848 _reflns_number_gt 4599 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'Bruker saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0752P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7848 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.236342(14) 0.63267(4) 0.146130(17) 0.06422(17) Uani 1 1 d . . . Fe1 Fe 0.5000 0.81924(7) 0.2500 0.0336(2) Uani 1 2 d S . . N11 N 0.18862(14) 0.6749(3) 0.2136(2) 0.0542(11) Uani 1 1 d . . . C12 C 0.14842(19) 0.7066(4) 0.1958(3) 0.0655(16) Uani 1 1 d . . . H41 H 0.1381 0.7102 0.1519 0.079 Uiso 1 1 calc R . . C13 C 0.12100(19) 0.7346(4) 0.2380(3) 0.0689(17) Uani 1 1 d . . . H27 H 0.0918 0.7551 0.2238 0.083 Uiso 1 1 calc R . . C14 C 0.1364(2) 0.7326(4) 0.3016(3) 0.0672(16) Uani 1 1 d . . . H33 H 0.1184 0.7537 0.3318 0.081 Uiso 1 1 calc R . . C15 C 0.17767(19) 0.7001(4) 0.3203(3) 0.0556(14) Uani 1 1 d . . . H36 H 0.1887 0.6977 0.3640 0.067 Uiso 1 1 calc R . . C16 C 0.20373(17) 0.6704(4) 0.2756(2) 0.0504(13) Uani 1 1 d . . . N21 N 0.26620(13) 0.5766(3) 0.25151(18) 0.0471(10) Uani 1 1 d . . . C22 C 0.24734(16) 0.6278(4) 0.2940(2) 0.0451(11) Uani 1 1 d . . . C23 C 0.27332(18) 0.6277(4) 0.3531(2) 0.0526(13) Uani 1 1 d . . . H5 H 0.2675 0.6586 0.3910 0.063 Uiso 1 1 calc R . . C24 C 0.30905(19) 0.5727(4) 0.3436(2) 0.0547(14) Uani 1 1 d . . . H44 H 0.3333 0.5576 0.3744 0.066 Uiso 1 1 calc R . . N25 N 0.30366(14) 0.5437(3) 0.28252(18) 0.0494(10) Uani 1 1 d . . . C26 C 0.33361(18) 0.4876(4) 0.2483(2) 0.0566(14) Uani 1 1 d . . . H12A H 0.3163 0.4405 0.2203 0.068 Uiso 1 1 calc R . . H12B H 0.3540 0.4505 0.2792 0.068 Uiso 1 1 calc R . . C31 C 0.36003(16) 0.5505(4) 0.2091(2) 0.0454(12) Uani 1 1 d . . . C32 C 0.38693(17) 0.5069(4) 0.1705(2) 0.0523(13) Uani 1 1 d . . . H20 H 0.3879 0.4381 0.1683 0.063 Uiso 1 1 calc R . . C33 C 0.41206(18) 0.5600(4) 0.1354(2) 0.0551(14) Uani 1 1 d . . . H17 H 0.4307 0.5284 0.1095 0.066 Uiso 1 1 calc R . . C34 C 0.41049(16) 0.6613(4) 0.1373(2) 0.0485(13) Uani 1 1 d . . . C35 C 0.38314(15) 0.7053(4) 0.1743(2) 0.0445(12) Uani 1 1 d . . . H22 H 0.3813 0.7741 0.1751 0.053 Uiso 1 1 calc R . . C36 C 0.35804(16) 0.6505(4) 0.2108(2) 0.0483(12) Uani 1 1 d . . . H6 H 0.3395 0.6819 0.2368 0.058 Uiso 1 1 calc R . . N41 N 0.46165(12) 0.8622(3) 0.15906(17) 0.0457(9) Uani 1 1 d . . . C42 C 0.45724(18) 0.9578(4) 0.1511(3) 0.0606(15) Uani 1 1 d . . . C43 C 0.4305(2) 0.9761(6) 0.0927(3) 0.089(2) Uani 1 1 d . . . H29 H 0.4216 1.0376 0.0755 0.106 Uiso 1 1 calc R . . C44 C 0.4203(2) 0.8872(6) 0.0663(3) 0.080(2) Uani 1 1 d . . . H39 H 0.4029 0.8748 0.0269 0.096 Uiso 1 1 calc R . . N45 N 0.43969(14) 0.8209(4) 0.10665(18) 0.0576(12) Uani 1 1 d . . . C46 C 0.43944(18) 0.7166(4) 0.0963(2) 0.0564(14) Uani 1 1 d . . . H8A H 0.4699 0.6919 0.1052 0.068 Uiso 1 1 calc R . . H8B H 0.4289 0.7034 0.0512 0.068 Uiso 1 1 calc R . . N51 N 0.5000 0.9730(4) 0.2500 0.0505(15) Uani 1 2 d S . . C52 C 0.47876(18) 1.0207(4) 0.2000(3) 0.0634(16) Uani 1 1 d . . . C53 C 0.4783(2) 1.1232(5) 0.1996(4) 0.095(2) Uani 1 1 d . . . H53 H 0.4632 1.1573 0.1647 0.114 Uiso 1 1 calc R . . C54 C 0.5000 1.1733(2) 0.2500 0.114(4) Uiso 1 2 d S . . H54 H 0.5000 1.2423 0.2500 0.137 Uiso 1 2 calc SR . . N61 N 0.5000 0.6663(2) 0.2500 0.0370(12) Uani 1 2 d SR . . C62 C 0.5249 0.6197(2) 0.2137 0.0444(12) Uani 1 1 d R . . C63 C 0.5248 0.5193(2) 0.2113 0.0630(15) Uani 1 1 d R . . H4 H 0.5415 0.4855 0.1837 0.076 Uiso 1 1 calc R . . C64 C 0.5000 0.4701(6) 0.2500 0.077(3) Uani 1 2 d S . . H1 H 0.5000 0.4012 0.2500 0.092 Uiso 1 2 calc SR . . N71 N 0.55410(12) 0.7769(3) 0.19218(15) 0.0374(9) Uani 1 1 d . . . C72 C 0.55137(15) 0.6820(4) 0.1779(2) 0.0436(12) Uani 1 1 d . . . C73 C 0.57610(18) 0.6591(4) 0.1292(2) 0.0554(14) Uani 1 1 d . . . H26 H 0.5793 0.5975 0.1103 0.067 Uiso 1 1 calc R . . C74 C 0.59450(18) 0.7449(4) 0.1149(2) 0.0573(14) Uani 1 1 d . . . H19 H 0.6136 0.7547 0.0838 0.069 Uiso 1 1 calc R . . N75 N 0.58063(13) 0.8134(3) 0.15271(17) 0.0442(10) Uani 1 1 d . . . C76 C 0.59787(17) 0.9136(4) 0.1605(2) 0.0506(13) Uani 1 1 d . . . H10A H 0.5741 0.9579 0.1695 0.061 Uiso 1 1 calc R . . H10B H 0.6084 0.9352 0.1208 0.061 Uiso 1 1 calc R . . C81 C 0.63562(16) 0.9177(4) 0.2146(2) 0.0433(11) Uani 1 1 d . . . C82 C 0.67421(16) 0.8682(4) 0.2117(2) 0.0475(12) Uani 1 1 d . . . H21 H 0.6789 0.8363 0.1737 0.057 Uiso 1 1 calc R . . C83 C 0.70642(16) 0.8644(4) 0.2640(2) 0.0505(12) Uani 1 1 d . . . H18 H 0.7329 0.8296 0.2615 0.061 Uiso 1 1 calc R . . C84 C 0.70017(16) 0.9109(4) 0.3195(2) 0.0512(13) Uani 1 1 d . . . C85 C 0.66229(17) 0.9647(4) 0.3223(2) 0.0497(12) Uani 1 1 d . . . H25 H 0.6582 0.9989 0.3598 0.060 Uiso 1 1 calc R . . C86 C 0.62996(16) 0.9681(4) 0.2692(2) 0.0463(12) Uani 1 1 d . . . H38 H 0.6040 1.0052 0.2708 0.056 Uiso 1 1 calc R . . N91 N 0.26904(14) 0.5359(3) 0.07757(17) 0.0495(11) Uani 1 1 d . . . C92 C 0.26758(19) 0.4372(4) 0.0770(2) 0.0591(15) Uani 1 1 d . . . H45 H 0.2473 0.4059 0.1004 0.071 Uiso 1 1 calc R . . C93 C 0.2935(2) 0.3811(4) 0.0449(2) 0.0640(16) Uani 1 1 d . . . H2 H 0.2909 0.3124 0.0451 0.077 Uiso 1 1 calc R . . C94 C 0.3237(2) 0.4257(5) 0.0119(2) 0.0633(16) Uani 1 1 d . . . H28 H 0.3429 0.3884 -0.0101 0.076 Uiso 1 1 calc R . . C95 C 0.32539(19) 0.5265(4) 0.0116(2) 0.0566(14) Uani 1 1 d . . . H43 H 0.3455 0.5591 -0.0115 0.068 Uiso 1 1 calc R . . C96 C 0.29798(17) 0.5788(4) 0.0447(2) 0.0471(13) Uani 1 1 d . . . N101 N 0.27773(13) 0.7324(3) 0.08888(18) 0.0473(10) Uani 1 1 d . . . C102 C 0.29847(16) 0.6854(4) 0.0470(2) 0.0453(12) Uani 1 1 d . . . C103 C 0.31792(18) 0.7526(4) 0.0097(2) 0.0535(14) Uani 1 1 d . . . H13 H 0.3349 0.7393 -0.0235 0.064 Uiso 1 1 calc R . . C104 C 0.30721(18) 0.8405(4) 0.0315(3) 0.0568(15) Uani 1 1 d . . . H42 H 0.3156 0.9015 0.0160 0.068 Uiso 1 1 calc R . . N105 N 0.28301(13) 0.8276(3) 0.07812(19) 0.0492(11) Uani 1 1 d . . . C106 C 0.26786(18) 0.8995(4) 0.1200(3) 0.0587(14) Uani 1 1 d . . . H34A H 0.2387 0.8799 0.1309 0.070 Uiso 1 1 calc R . . H34B H 0.2644 0.9627 0.0979 0.070 Uiso 1 1 calc R . . B1 B 0.0805(3) 0.8609(6) 0.0846(3) 0.076(2) Uani 1 1 d . . . F1A F 0.0593(2) 0.9160(3) 0.0363(2) 0.140(2) Uani 1 1 d . . . F1B F 0.1160(2) 0.9082(4) 0.1127(2) 0.153(2) Uani 1 1 d . . . F1C F 0.05305(16) 0.8416(3) 0.12932(18) 0.1052(14) Uani 1 1 d . . . F1D F 0.09201(11) 0.7754(3) 0.05969(13) 0.0717(10) Uani 1 1 d . . . B2 B 0.1602(2) 0.3716(5) 0.9996(3) 0.0541(15) Uani 1 1 d . . . F2A F 0.12579(12) 0.3243(3) 0.96381(17) 0.0829(11) Uani 1 1 d . . . F2B F 0.19106(11) 0.3986(2) 0.96094(12) 0.0643(8) Uani 1 1 d . . . F2C F 0.17921(10) 0.3090(2) 1.04630(13) 0.0627(8) Uani 1 1 d . . . F2D F 0.14541(13) 0.4532(3) 1.02631(16) 0.0842(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0548(2) 0.0905(4) 0.0467(2) -0.0061(2) 0.00438(16) -0.0041(2) Fe1 0.0387(6) 0.0276(5) 0.0336(5) 0.000 0.0013(4) 0.000 N11 0.042(2) 0.063(3) 0.058(2) 0.002(2) 0.011(2) -0.003(2) C12 0.055(4) 0.067(4) 0.073(4) 0.017(3) 0.004(3) -0.005(3) C13 0.050(3) 0.059(4) 0.101(5) 0.016(3) 0.020(3) 0.008(3) C14 0.070(4) 0.043(4) 0.093(4) 0.005(3) 0.030(4) -0.005(3) C15 0.063(4) 0.041(3) 0.066(3) -0.002(3) 0.022(3) -0.004(3) C16 0.055(3) 0.042(3) 0.056(3) 0.003(2) 0.014(3) -0.003(2) N21 0.046(2) 0.049(3) 0.046(2) 0.0008(19) 0.0030(19) -0.003(2) C22 0.051(3) 0.038(3) 0.049(2) 0.005(2) 0.014(2) -0.004(2) C23 0.071(4) 0.045(3) 0.043(2) -0.005(2) 0.012(2) -0.002(3) C24 0.063(4) 0.058(4) 0.042(3) 0.006(2) 0.001(2) -0.003(3) N25 0.055(3) 0.045(3) 0.049(2) 0.0015(19) 0.010(2) 0.000(2) C26 0.057(3) 0.060(4) 0.053(3) -0.003(3) 0.009(3) 0.007(3) C31 0.043(3) 0.046(3) 0.045(2) -0.003(2) 0.001(2) 0.000(2) C32 0.058(3) 0.050(3) 0.050(3) -0.008(3) 0.009(3) 0.000(3) C33 0.061(4) 0.062(4) 0.043(3) -0.009(3) 0.009(2) 0.006(3) C34 0.044(3) 0.067(4) 0.033(2) -0.001(2) -0.001(2) -0.003(3) C35 0.043(3) 0.046(3) 0.043(2) -0.002(2) -0.003(2) 0.000(2) C36 0.046(3) 0.053(4) 0.044(2) -0.003(2) -0.001(2) 0.002(3) N41 0.042(2) 0.048(3) 0.0456(19) 0.0146(19) 0.0000(17) 0.000(2) C42 0.049(3) 0.055(4) 0.079(4) 0.032(3) 0.013(3) 0.007(3) C43 0.066(4) 0.112(6) 0.089(5) 0.068(5) 0.013(3) 0.028(4) C44 0.067(4) 0.097(6) 0.073(4) 0.040(4) -0.007(3) 0.002(4) N45 0.049(3) 0.079(4) 0.042(2) 0.022(2) -0.0060(19) -0.002(2) C46 0.058(3) 0.074(4) 0.034(2) 0.002(3) -0.007(2) -0.006(3) N51 0.049(4) 0.024(3) 0.081(4) 0.000 0.017(3) 0.000 C52 0.047(3) 0.039(3) 0.107(5) 0.023(3) 0.021(3) 0.006(3) C53 0.067(4) 0.059(5) 0.164(7) 0.047(5) 0.036(4) 0.022(3) N61 0.039(3) 0.037(3) 0.033(2) 0.000 -0.004(2) 0.000 C62 0.047(3) 0.037(3) 0.047(2) -0.008(2) -0.004(2) 0.007(2) C63 0.071(4) 0.042(4) 0.075(4) -0.017(3) 0.005(3) 0.009(3) C64 0.104(7) 0.024(4) 0.103(7) 0.000 0.015(6) 0.000 N71 0.040(2) 0.040(2) 0.0320(17) 0.0021(16) 0.0029(16) -0.0017(18) C72 0.041(3) 0.047(3) 0.040(2) -0.009(2) -0.003(2) 0.003(2) C73 0.063(3) 0.054(4) 0.051(3) -0.019(3) 0.013(3) 0.003(3) C74 0.056(3) 0.067(4) 0.050(3) -0.013(3) 0.013(2) 0.004(3) N75 0.047(2) 0.048(3) 0.0375(19) 0.0026(19) 0.0050(18) -0.005(2) C76 0.048(3) 0.056(4) 0.050(3) 0.006(2) 0.011(2) -0.003(3) C81 0.047(3) 0.040(3) 0.043(2) 0.006(2) 0.009(2) -0.010(2) C82 0.045(3) 0.044(3) 0.055(3) 0.006(2) 0.008(2) -0.009(2) C83 0.047(3) 0.040(3) 0.064(3) 0.007(3) 0.006(2) -0.004(2) C84 0.043(3) 0.042(3) 0.066(3) 0.007(3) -0.004(2) -0.011(2) C85 0.052(3) 0.041(3) 0.055(3) 0.000(2) 0.001(2) -0.005(2) C86 0.044(3) 0.038(3) 0.056(3) 0.003(2) 0.002(2) -0.003(2) N91 0.054(3) 0.053(3) 0.038(2) -0.010(2) -0.0044(19) -0.004(2) C92 0.065(4) 0.058(4) 0.050(3) 0.001(3) -0.008(3) -0.010(3) C93 0.090(4) 0.052(4) 0.045(3) -0.007(3) -0.008(3) 0.000(3) C94 0.077(4) 0.066(4) 0.043(3) 0.000(3) -0.006(3) 0.011(3) C95 0.062(3) 0.067(4) 0.038(2) 0.004(3) -0.003(2) 0.001(3) C96 0.047(3) 0.056(3) 0.034(2) 0.001(2) -0.010(2) 0.004(3) N101 0.044(2) 0.047(3) 0.048(2) 0.003(2) -0.0035(19) -0.004(2) C102 0.040(3) 0.054(3) 0.039(2) 0.005(2) -0.008(2) 0.001(2) C103 0.059(3) 0.056(4) 0.041(2) 0.004(3) -0.010(2) 0.003(3) C104 0.054(3) 0.054(4) 0.056(3) 0.011(3) -0.016(3) -0.005(3) N105 0.044(2) 0.048(3) 0.052(2) 0.001(2) -0.009(2) 0.003(2) C106 0.051(3) 0.051(3) 0.069(3) -0.007(3) -0.010(3) 0.012(3) B1 0.101(6) 0.076(5) 0.050(3) -0.005(4) 0.006(4) 0.011(5) F1A 0.228(6) 0.096(3) 0.092(3) 0.015(3) 0.010(3) 0.058(4) F1B 0.213(6) 0.159(5) 0.082(3) -0.022(3) 0.004(3) -0.121(4) F1C 0.138(4) 0.103(3) 0.084(2) -0.010(2) 0.050(3) 0.024(3) F1D 0.083(2) 0.081(2) 0.0484(15) -0.0183(16) -0.0009(15) 0.0246(19) B2 0.064(4) 0.052(4) 0.047(3) 0.008(3) 0.009(3) 0.009(3) F2A 0.070(2) 0.087(3) 0.086(2) 0.017(2) -0.0102(18) -0.0128(19) F2B 0.076(2) 0.075(2) 0.0443(14) 0.0127(14) 0.0163(14) -0.0059(18) F2C 0.073(2) 0.063(2) 0.0526(16) 0.0237(14) 0.0097(14) 0.0086(16) F2D 0.120(3) 0.064(2) 0.075(2) 0.0159(18) 0.037(2) 0.030(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11 2.259(4) . ? Ag1 N91 2.304(4) . ? Ag1 N101 2.323(4) . ? Ag1 N21 2.440(4) . ? Fe1 N61 2.107(3) . ? Fe1 N51 2.118(6) . ? Fe1 N41 2.214(3) 2_655 ? Fe1 N41 2.214(3) . ? Fe1 N71 2.269(4) . ? Fe1 N71 2.269(4) 2_655 ? N11 C12 1.317(7) . ? N11 C16 1.344(6) . ? C12 C13 1.366(8) . ? C13 C14 1.377(8) . ? C14 C15 1.352(8) . ? C15 C16 1.383(8) . ? C16 C22 1.466(7) . ? N21 N25 1.329(5) . ? N21 C22 1.338(6) . ? C22 C23 1.401(6) . ? C23 C24 1.369(7) . ? C24 N25 1.351(6) . ? N25 C26 1.465(7) . ? C26 C31 1.511(7) . ? C31 C32 1.378(7) . ? C31 C36 1.381(7) . ? C32 C33 1.357(7) . ? C33 C34 1.398(8) . ? C34 C35 1.367(7) . ? C34 C46 1.529(7) . ? C35 C36 1.387(7) . ? N41 C42 1.333(7) . ? N41 N45 1.353(6) . ? C42 C43 1.421(8) . ? C42 C52 1.448(8) . ? C43 C44 1.367(10) . ? C44 N45 1.339(7) . ? N45 C46 1.455(7) . ? N51 C52 1.347(6) . ? N51 C52 1.347(6) 2_655 ? C52 C53 1.414(8) . ? C53 C54 1.374(9) . ? C54 C53 1.374(9) 2_655 ? N61 C62 1.3236 . ? N61 C62 1.3236 2_655 ? C62 C63 1.3843 . ? C62 C72 1.462(5) . ? C63 C64 1.373(4) . ? C64 C63 1.373(4) 2_655 ? N71 C72 1.343(6) . ? N71 N75 1.343(5) . ? C72 C73 1.401(7) . ? C73 C74 1.362(8) . ? C74 N75 1.346(6) . ? N75 C76 1.480(6) . ? C76 C81 1.525(6) . ? C81 C82 1.374(7) . ? C81 C86 1.387(7) . ? C82 C83 1.392(7) . ? C83 C84 1.381(8) . ? C84 C85 1.386(7) . ? C84 C106 1.524(7) 2_655 ? C85 C86 1.405(6) . ? N91 C96 1.339(7) . ? N91 C92 1.360(7) . ? C92 C93 1.358(8) . ? C93 C94 1.379(9) . ? C94 C95 1.390(8) . ? C95 C96 1.372(8) . ? C96 C102 1.470(7) . ? N101 C102 1.330(6) . ? N101 N105 1.345(6) . ? C102 C103 1.404(7) . ? C103 C104 1.354(8) . ? C104 N105 1.329(7) . ? N105 C106 1.451(7) . ? C106 C84 1.524(7) 2_655 ? B1 F1B 1.342(9) . ? B1 F1D 1.358(8) . ? B1 F1A 1.374(8) . ? B1 F1C 1.378(9) . ? B2 F2D 1.364(7) . ? B2 F2A 1.384(7) . ? B2 F2B 1.384(7) . ? B2 F2C 1.387(6) . ? 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 N91 157.76(16) . . ? N11 Ag1 N101 128.82(16) . . ? N91 Ag1 N101 72.28(16) . . ? N11 Ag1 N21 71.98(15) . . ? N91 Ag1 N21 105.05(14) . . ? N101 Ag1 N21 120.44(13) . . ? N61 Fe1 N51 180.000(1) . . ? N61 Fe1 N41 105.51(11) . 2_655 ? N51 Fe1 N41 74.49(11) . 2_655 ? N61 Fe1 N41 105.51(11) . . ? N51 Fe1 N41 74.49(11) . . ? N41 Fe1 N41 149.0(2) 2_655 . ? N61 Fe1 N71 75.08(10) . . ? N51 Fe1 N71 104.92(10) . . ? N41 Fe1 N71 101.70(13) 2_655 . ? N41 Fe1 N71 86.27(13) . . ? N61 Fe1 N71 75.08(10) . 2_655 ? N51 Fe1 N71 104.92(10) . 2_655 ? N41 Fe1 N71 86.27(13) 2_655 2_655 ? N41 Fe1 N71 101.70(13) . 2_655 ? N71 Fe1 N71 150.2(2) . 2_655 ? C12 N11 C16 119.3(5) . . ? C12 N11 Ag1 124.2(4) . . ? C16 N11 Ag1 116.5(3) . . ? N11 C12 C13 122.5(6) . . ? C12 C13 C14 118.8(6) . . ? C15 C14 C13 119.0(6) . . ? C14 C15 C16 119.8(6) . . ? N11 C16 C15 120.5(5) . . ? N11 C16 C22 117.8(4) . . ? C15 C16 C22 121.5(5) . . ? N25 N21 C22 105.4(4) . . ? N25 N21 Ag1 139.7(3) . . ? C22 N21 Ag1 108.3(3) . . ? N21 C22 C23 111.3(4) . . ? N21 C22 C16 119.3(4) . . ? C23 C22 C16 129.3(5) . . ? C24 C23 C22 103.8(4) . . ? N25 C24 C23 107.9(4) . . ? N21 N25 C24 111.6(4) . . ? N21 N25 C26 119.3(4) . . ? C24 N25 C26 129.0(4) . . ? N25 C26 C31 113.0(4) . . ? C32 C31 C36 118.8(5) . . ? C32 C31 C26 119.2(5) . . ? C36 C31 C26 122.0(5) . . ? C33 C32 C31 121.5(5) . . ? C32 C33 C34 119.9(5) . . ? C35 C34 C33 119.1(5) . . ? C35 C34 C46 123.8(5) . . ? C33 C34 C46 117.1(5) . . ? C34 C35 C36 120.7(5) . . ? C31 C36 C35 120.0(5) . . ? C42 N41 N45 106.2(4) . . ? C42 N41 Fe1 114.2(3) . . ? N45 N41 Fe1 139.6(3) . . ? N41 C42 C43 109.0(6) . . ? N41 C42 C52 118.0(4) . . ? C43 C42 C52 133.0(6) . . ? C44 C43 C42 106.1(6) . . ? N45 C44 C43 106.7(6) . . ? C44 N45 N41 112.1(5) . . ? C44 N45 C46 125.6(5) . . ? N41 N45 C46 122.2(4) . . ? N45 C46 C34 113.4(5) . . ? C52 N51 C52 121.6(7) . 2_655 ? C52 N51 Fe1 119.2(3) . . ? C52 N51 Fe1 119.2(3) 2_655 . ? N51 C52 C53 119.7(6) . . ? N51 C52 C42 114.0(5) . . ? C53 C52 C42 126.3(6) . . ? C54 C53 C52 119.7(6) . . ? C53 C54 C53 119.7(6) . 2_655 ? C62 N61 C62 121.9 . 2_655 ? C62 N61 Fe1 119.0 . . ? C62 N61 Fe1 119.0 2_655 . ? N61 C62 C63 120.6 . . ? N61 C62 C72 115.0(2) . . ? C63 C62 C72 124.4(2) . . ? C64 C63 C62 118.0(3) . . ? C63 C64 C63 120.9(6) . 2_655 ? C72 N71 N75 104.4(4) . . ? C72 N71 Fe1 110.2(3) . . ? N75 N71 Fe1 142.2(3) . . ? N71 C72 C73 111.3(5) . . ? N71 C72 C62 118.4(4) . . ? C73 C72 C62 130.3(5) . . ? C74 C73 C72 104.5(5) . . ? N75 C74 C73 107.6(5) . . ? N71 N75 C74 112.2(4) . . ? N71 N75 C76 121.1(4) . . ? C74 N75 C76 125.8(4) . . ? N75 C76 C81 110.1(4) . . ? C82 C81 C86 119.3(4) . . ? C82 C81 C76 121.4(4) . . ? C86 C81 C76 119.2(5) . . ? C81 C82 C83 120.5(5) . . ? C84 C83 C82 120.4(5) . . ? C83 C84 C85 119.8(4) . . ? C83 C84 C106 122.2(5) . 2_655 ? C85 C84 C106 117.9(5) . 2_655 ? C84 C85 C86 119.3(5) . . ? C81 C86 C85 120.5(5) . . ? C96 N91 C92 117.4(5) . . ? C96 N91 Ag1 116.7(3) . . ? C92 N91 Ag1 124.6(4) . . ? C93 C92 N91 123.6(6) . . ? C92 C93 C94 118.7(6) . . ? C93 C94 C95 118.4(6) . . ? C96 C95 C94 119.8(6) . . ? N91 C96 C95 122.0(5) . . ? N91 C96 C102 115.4(5) . . ? C95 C96 C102 122.6(5) . . ? C102 N101 N105 106.3(4) . . ? C102 N101 Ag1 114.1(3) . . ? N105 N101 Ag1 138.8(4) . . ? N101 C102 C103 109.6(5) . . ? N101 C102 C96 120.3(5) . . ? C103 C102 C96 130.1(5) . . ? C104 C103 C102 104.8(5) . . ? N105 C104 C103 108.7(5) . . ? C104 N105 N101 110.5(5) . . ? C104 N105 C106 128.6(5) . . ? N101 N105 C106 120.4(5) . . ? N105 C106 C84 111.7(4) . 2_655 ? F1B B1 F1D 111.1(7) . . ? F1B B1 F1A 110.0(7) . . ? F1D B1 F1A 108.0(5) . . ? F1B B1 F1C 108.4(6) . . ? F1D B1 F1C 108.5(7) . . ? F1A B1 F1C 110.8(7) . . ? F2D B2 F2A 110.3(5) . . ? F2D B2 F2B 108.6(5) . . ? F2A B2 F2B 109.2(4) . . ? F2D B2 F2C 110.1(4) . . ? F2A B2 F2C 108.7(5) . . ? F2B B2 F2C 109.9(5) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 70.43 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.229 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.082 #===END data_Ag3 _database_code_depnum_ccdc_archive 'CCDC 265435' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C86 H70 Ag3 N22, C H3 N O2, 3(B F4)' _chemical_formula_sum 'C87 H73 Ag3 B3 F12 N23 O2' _chemical_formula_weight 2056.72 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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 28.943(5) _cell_length_b 11.5611(19) _cell_length_c 25.405(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.848(3) _cell_angle_gamma 90.00 _cell_volume 8349(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6791 _cell_measurement_theta_min 4.540 _cell_measurement_theta_max 46.463 _exptl_crystal_description BLOCK _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6936 _exptl_absorpt_correction_T_max 0.8581 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 67846 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 23.31 _reflns_number_total 12038 _reflns_number_gt 9248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+8.9597P] 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 12038 _refine_ls_number_parameters 1172 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.477660(13) 0.72555(3) 0.493914(14) 0.04230(11) Uani 1 1 d . . . Ag2 Ag 0.229462(12) 0.72280(3) 0.272364(13) 0.03419(11) Uani 1 1 d . . . Ag3 Ag 0.075628(14) 0.89633(3) -0.015018(14) 0.04602(12) Uani 1 1 d . . . N111 N 0.50795(12) 0.6137(3) 0.43423(13) 0.0331(8) Uani 1 1 d . . . C112 C 0.48091(15) 0.5250(3) 0.41216(16) 0.0303(10) Uani 1 1 d . . . C113 C 0.48846(16) 0.4698(4) 0.36618(17) 0.0387(11) Uani 1 1 d . . . H113 H 0.4689 0.4074 0.3515 0.046 Uiso 1 1 calc R . . C114 C 0.52476(17) 0.5064(4) 0.34190(19) 0.0473(12) Uani 1 1 d . . . H114 H 0.5302 0.4702 0.3101 0.057 Uiso 1 1 calc R . . C115 C 0.55283(17) 0.5958(4) 0.36433(19) 0.0464(12) Uani 1 1 d . . . H115 H 0.5783 0.6219 0.3487 0.056 Uiso 1 1 calc R . . C116 C 0.54330(16) 0.6469(4) 0.41014(18) 0.0387(11) Uani 1 1 d . . . H116 H 0.5628 0.7090 0.4255 0.046 Uiso 1 1 calc R . . N121 N 0.42766(12) 0.5605(3) 0.47361(13) 0.0322(8) Uani 1 1 d . . . N122 N 0.39137(12) 0.5045(3) 0.48897(13) 0.0345(9) Uani 1 1 d . . . C123 C 0.38221(16) 0.4022(4) 0.46343(17) 0.0389(11) Uani 1 1 d . . . H123 H 0.3581 0.3492 0.4675 0.047 Uiso 1 1 calc R . . C124 C 0.41442(16) 0.3895(4) 0.43046(18) 0.0378(11) Uani 1 1 d . . . H124 H 0.4175 0.3261 0.4076 0.045 Uiso 1 1 calc R . . C125 C 0.44178(14) 0.4905(3) 0.43790(15) 0.0296(10) Uani 1 1 d . . . C131 C 0.36327(16) 0.5635(4) 0.52308(17) 0.0399(11) Uani 1 1 d . . . H13A H 0.3844 0.5987 0.5541 0.048 Uiso 1 1 calc R . . H13B H 0.3430 0.5065 0.5370 0.048 Uiso 1 1 calc R . . C132 C 0.33291(15) 0.6564(4) 0.49221(15) 0.0307(10) Uani 1 1 d . . . C133 C 0.34360(14) 0.7735(4) 0.50093(16) 0.0322(10) Uani 1 1 d . . . H133 H 0.3694 0.7954 0.5281 0.039 Uiso 1 1 calc R . . C134 C 0.31724(14) 0.8580(4) 0.47059(16) 0.0329(10) Uani 1 1 d . . . H134 H 0.3251 0.9372 0.4770 0.039 Uiso 1 1 calc R . . C135 C 0.27923(14) 0.8277(4) 0.43068(15) 0.0280(9) Uani 1 1 d . . . C136 C 0.26772(15) 0.7116(4) 0.42252(16) 0.0316(10) Uani 1 1 d . . . H136 H 0.2416 0.6901 0.3957 0.038 Uiso 1 1 calc R . . C137 C 0.29412(15) 0.6268(4) 0.45333(16) 0.0347(10) Uani 1 1 d . . . H137 H 0.2856 0.5477 0.4478 0.042 Uiso 1 1 calc R . . C138 C 0.25113(15) 0.9196(4) 0.39671(16) 0.0311(10) Uani 1 1 d . . . H13C H 0.2195 0.8889 0.3815 0.037 Uiso 1 1 calc R . . H13D H 0.2471 0.9869 0.4195 0.037 Uiso 1 1 calc R . . N141 N 0.27643(11) 0.8843(3) 0.31212(12) 0.0260(8) Uani 1 1 d . . . N142 N 0.27421(11) 0.9573(3) 0.35287(13) 0.0284(8) Uani 1 1 d . . . C143 C 0.29823(17) 1.0556(4) 0.34880(18) 0.0405(11) Uani 1 1 d . . . H143 H 0.3019 1.1188 0.3731 0.049 Uiso 1 1 calc R . . C144 C 0.31638(17) 1.0468(4) 0.30284(17) 0.0428(12) Uani 1 1 d . . . H144 H 0.3349 1.1023 0.2887 0.051 Uiso 1 1 calc R . . C145 C 0.30181(14) 0.9388(3) 0.28135(15) 0.0281(9) Uani 1 1 d . . . N151 N 0.28409(11) 0.7875(3) 0.21698(12) 0.0270(8) Uani 1 1 d . . . C152 C 0.31150(14) 0.8799(4) 0.23352(16) 0.0300(10) Uani 1 1 d . . . C153 C 0.34809(16) 0.9119(4) 0.20799(16) 0.0395(11) Uani 1 1 d . . . H153 H 0.3671 0.9772 0.2200 0.047 Uiso 1 1 calc R . . C154 C 0.35625(16) 0.8480(5) 0.16528(17) 0.0467(13) Uani 1 1 d . . . H154 H 0.3812 0.8686 0.1475 0.056 Uiso 1 1 calc R . . C155 C 0.32833(16) 0.7539(4) 0.14809(18) 0.0422(12) Uani 1 1 d . . . H155 H 0.3337 0.7088 0.1186 0.051 Uiso 1 1 calc R . . C156 C 0.29201(14) 0.7261(4) 0.17489(16) 0.0310(10) Uani 1 1 d . . . N161 N 0.22342(12) 0.6115(3) 0.18266(13) 0.0314(8) Uani 1 1 d . . . N162 N 0.20408(13) 0.5097(3) 0.16420(14) 0.0378(9) Uani 1 1 d . . . C163 C 0.22848(19) 0.4602(4) 0.12973(19) 0.0513(13) Uani 1 1 d . . . H163 H 0.2211 0.3893 0.1112 0.062 Uiso 1 1 calc R . . C164 C 0.26555(18) 0.5304(4) 0.12626(19) 0.0477(13) Uani 1 1 d . . . H164 H 0.2892 0.5186 0.1054 0.057 Uiso 1 1 calc R . . C165 C 0.26129(15) 0.6250(4) 0.16052(16) 0.0325(10) Uani 1 1 d . . . C171 C 0.16074(16) 0.4723(4) 0.17987(18) 0.0402(11) Uani 1 1 d . . . H17A H 0.1649 0.4735 0.2194 0.048 Uiso 1 1 calc R . . H17B H 0.1538 0.3917 0.1677 0.048 Uiso 1 1 calc R . . C172 C 0.11952(15) 0.5489(4) 0.15624(17) 0.0339(10) Uani 1 1 d . . . C173 C 0.08455(16) 0.5728(4) 0.18523(17) 0.0383(11) Uani 1 1 d . . . H173 H 0.0865 0.5412 0.2201 0.046 Uiso 1 1 calc R . . C174 C 0.04662(17) 0.6427(4) 0.16368(18) 0.0418(12) Uani 1 1 d . . . H174 H 0.0233 0.6597 0.1843 0.050 Uiso 1 1 calc R . . C175 C 0.04230(16) 0.6879(4) 0.11253(18) 0.0399(11) Uani 1 1 d . . . C176 C 0.07689(17) 0.6620(4) 0.08329(18) 0.0412(11) Uani 1 1 d . . . H176 H 0.0740 0.6905 0.0477 0.049 Uiso 1 1 calc R . . C177 C 0.11547(16) 0.5954(4) 0.10506(17) 0.0382(11) Uani 1 1 d . . . H177 H 0.1394 0.5812 0.0849 0.046 Uiso 1 1 calc R . . C178 C 0.00227(16) 0.7671(4) 0.0894(2) 0.0465(12) Uani 1 1 d . . . H17C H -0.0082 0.7497 0.0508 0.056 Uiso 1 1 calc R . . H17D H -0.0246 0.7532 0.1077 0.056 Uiso 1 1 calc R . . N181 N 0.03933(13) 0.9390(3) 0.06037(14) 0.0385(9) Uani 1 1 d . . . N182 N 0.01633(13) 0.8881(3) 0.09574(15) 0.0408(9) Uani 1 1 d . . . C183 C 0.01459(16) 0.9565(4) 0.13809(19) 0.0441(12) Uani 1 1 d . . . H183 H 0.0005 0.9382 0.1680 0.053 Uiso 1 1 calc R . . C184 C 0.03703(16) 1.0578(4) 0.12997(18) 0.0407(11) Uani 1 1 d . . . H184 H 0.0414 1.1238 0.1526 0.049 Uiso 1 1 calc R . . C185 C 0.05198(15) 1.0431(4) 0.08123(17) 0.0353(10) Uani 1 1 d . . . N191 N 0.09192(13) 1.0855(3) 0.00863(14) 0.0397(9) Uani 1 1 d . . . C192 C 0.07878(15) 1.1235(4) 0.05373(17) 0.0362(11) Uani 1 1 d . . . C193 C 0.09105(18) 1.2329(4) 0.0739(2) 0.0515(13) Uani 1 1 d . . . H193 H 0.0818 1.2581 0.1060 0.062 Uiso 1 1 calc R . . C194 C 0.1167(2) 1.3045(5) 0.0474(2) 0.0628(16) Uani 1 1 d . . . H194 H 0.1243 1.3805 0.0603 0.075 Uiso 1 1 calc R . . C195 C 0.1314(2) 1.2654(5) 0.0016(2) 0.0585(15) Uani 1 1 d . . . H195 H 0.1498 1.3128 -0.0170 0.070 Uiso 1 1 calc R . . C196 C 0.11817(17) 1.1556(4) -0.01596(19) 0.0471(12) Uani 1 1 d . . . H196 H 0.1282 1.1278 -0.0472 0.056 Uiso 1 1 calc R . . N211 N 0.46474(12) 0.8559(3) 0.55643(14) 0.0343(8) Uani 1 1 d . . . C212 C 0.44085(15) 0.9529(4) 0.53848(17) 0.0324(10) Uani 1 1 d . . . C213 C 0.42049(17) 1.0237(4) 0.5719(2) 0.0446(12) Uani 1 1 d . . . H213 H 0.4028 1.0897 0.5580 0.053 Uiso 1 1 calc R . . C214 C 0.42637(18) 0.9968(4) 0.6257(2) 0.0527(14) Uani 1 1 d . . . H214 H 0.4127 1.0443 0.6493 0.063 Uiso 1 1 calc R . . C215 C 0.45225(18) 0.9003(4) 0.6450(2) 0.0503(13) Uani 1 1 d . . . H215 H 0.4575 0.8812 0.6820 0.060 Uiso 1 1 calc R . . C216 C 0.47033(17) 0.8324(4) 0.60908(18) 0.0429(12) Uani 1 1 d . . . H216 H 0.4877 0.7653 0.6223 0.051 Uiso 1 1 calc R . . N221 N 0.45378(12) 0.9060(3) 0.44927(14) 0.0330(8) Uani 1 1 d . . . N222 N 0.44372(12) 0.9532(3) 0.39968(14) 0.0344(9) Uani 1 1 d . . . C223 C 0.41988(16) 1.0536(4) 0.4003(2) 0.0449(12) Uani 1 1 d . . . H223 H 0.4089 1.1020 0.3703 0.054 Uiso 1 1 calc R . . C224 C 0.41438(17) 1.0730(4) 0.4516(2) 0.0460(12) Uani 1 1 d . . . H224 H 0.3992 1.1368 0.4647 0.055 Uiso 1 1 calc R . . C225 C 0.43586(15) 0.9787(4) 0.48080(17) 0.0331(10) Uani 1 1 d . . . C231 C 0.45519(15) 0.8921(4) 0.35417(17) 0.0367(11) Uani 1 1 d . . . H23A H 0.4882 0.8652 0.3634 0.044 Uiso 1 1 calc R . . H23B H 0.4529 0.9466 0.3238 0.044 Uiso 1 1 calc R . . C232 C 0.42370(15) 0.7884(4) 0.33628(16) 0.0313(10) Uani 1 1 d . . . C233 C 0.38599(15) 0.7580(4) 0.35933(17) 0.0354(11) Uani 1 1 d . . . H233 H 0.3788 0.8026 0.3881 0.043 Uiso 1 1 calc R . . C234 C 0.35834(15) 0.6627(4) 0.34096(16) 0.0342(10) Uani 1 1 d . . . H234 H 0.3327 0.6427 0.3577 0.041 Uiso 1 1 calc R . . C235 C 0.36724(14) 0.5971(3) 0.29921(16) 0.0280(9) Uani 1 1 d . . . C236 C 0.40550(17) 0.6278(4) 0.27632(18) 0.0443(12) Uani 1 1 d . . . H236 H 0.4128 0.5827 0.2477 0.053 Uiso 1 1 calc R . . C237 C 0.43313(17) 0.7220(4) 0.29424(19) 0.0457(12) Uani 1 1 d . . . H237 H 0.4589 0.7415 0.2776 0.055 Uiso 1 1 calc R . . C238 C 0.33803(14) 0.4945(4) 0.27638(17) 0.0334(10) Uani 1 1 d . . . H23C H 0.3230 0.5125 0.2390 0.040 Uiso 1 1 calc R . . H23D H 0.3593 0.4278 0.2753 0.040 Uiso 1 1 calc R . . N241 N 0.26166(11) 0.5218(3) 0.30146(13) 0.0286(8) Uani 1 1 d . . . N242 N 0.30148(11) 0.4602(3) 0.30559(13) 0.0296(8) Uani 1 1 d . . . C243 C 0.30068(16) 0.3651(4) 0.33564(18) 0.0407(11) Uani 1 1 d . . . H243 H 0.3249 0.3088 0.3436 0.049 Uiso 1 1 calc R . . C244 C 0.25857(16) 0.3640(4) 0.35269(19) 0.0432(12) Uani 1 1 d . . . H244 H 0.2476 0.3080 0.3748 0.052 Uiso 1 1 calc R . . C245 C 0.23515(14) 0.4635(3) 0.33042(16) 0.0295(10) Uani 1 1 d . . . N251 N 0.17669(11) 0.6145(3) 0.31576(12) 0.0254(8) Uani 1 1 d . . . C252 C 0.18777(14) 0.5057(3) 0.33392(15) 0.0274(9) Uani 1 1 d . . . C253 C 0.15577(15) 0.4361(4) 0.35363(17) 0.0381(11) Uani 1 1 d . . . H253 H 0.1641 0.3601 0.3662 0.046 Uiso 1 1 calc R . . C254 C 0.11167(16) 0.4798(4) 0.35460(17) 0.0405(12) Uani 1 1 d . . . H254 H 0.0891 0.4335 0.3676 0.049 Uiso 1 1 calc R . . C255 C 0.10016(15) 0.5907(4) 0.33668(17) 0.0361(11) Uani 1 1 d . . . H255 H 0.0699 0.6217 0.3374 0.043 Uiso 1 1 calc R . . C256 C 0.13358(14) 0.6558(4) 0.31759(15) 0.0279(9) Uani 1 1 d . . . N261 N 0.15821(11) 0.8437(3) 0.28919(13) 0.0297(8) Uani 1 1 d . . . N262 N 0.13646(12) 0.9437(3) 0.27031(13) 0.0329(8) Uani 1 1 d . . . C263 C 0.08964(15) 0.9362(4) 0.26546(17) 0.0402(11) Uani 1 1 d . . . H263 H 0.0675 0.9951 0.2527 0.048 Uiso 1 1 calc R . . C264 C 0.07963(15) 0.8291(4) 0.28218(17) 0.0393(11) Uani 1 1 d . . . H264 H 0.0495 0.7981 0.2837 0.047 Uiso 1 1 calc R . . C265 C 0.12340(14) 0.7740(4) 0.29675(15) 0.0298(10) Uani 1 1 d . . . C271 C 0.16372(16) 1.0355(4) 0.25128(17) 0.0375(11) Uani 1 1 d . . . H27A H 0.1939 1.0447 0.2767 0.045 Uiso 1 1 calc R . . H27B H 0.1462 1.1093 0.2505 0.045 Uiso 1 1 calc R . . C272 C 0.17371(15) 1.0111(4) 0.19584(16) 0.0338(10) Uani 1 1 d . . . C273 C 0.16210(16) 0.9097(4) 0.16901(18) 0.0401(11) Uani 1 1 d . . . H273 H 0.1452 0.8526 0.1845 0.048 Uiso 1 1 calc R . . C274 C 0.17439(16) 0.8883(4) 0.11997(18) 0.0417(11) Uani 1 1 d . . . H274 H 0.1662 0.8163 0.1027 0.050 Uiso 1 1 calc R . . C275 C 0.19821(15) 0.9693(4) 0.09563(17) 0.0378(11) Uani 1 1 d . . . C276 C 0.2079(2) 1.0738(5) 0.1215(2) 0.0710(18) Uani 1 1 d . . . H276 H 0.2231 1.1331 0.1052 0.085 Uiso 1 1 calc R . . C277 C 0.1960(2) 1.0935(5) 0.1707(2) 0.0696(18) Uani 1 1 d . . . H277 H 0.2033 1.1661 0.1878 0.084 Uiso 1 1 calc R . . C278 C 0.21457(17) 0.9481(4) 0.04355(18) 0.0463(12) Uani 1 1 d . . . H27C H 0.2016 1.0090 0.0176 0.056 Uiso 1 1 calc R . . H27D H 0.2493 0.9536 0.0498 0.056 Uiso 1 1 calc R . . N281 N 0.15716(13) 0.8217(3) -0.01014(14) 0.0390(9) Uani 1 1 d . . . N282 N 0.20016(13) 0.8352(3) 0.02065(14) 0.0396(9) Uani 1 1 d . . . C283 C 0.22310(17) 0.7339(5) 0.02907(18) 0.0444(12) Uani 1 1 d . . . H283 H 0.2537 0.7229 0.0497 0.053 Uiso 1 1 calc R . . C284 C 0.19474(16) 0.6497(4) 0.00279(17) 0.0407(11) Uani 1 1 d . . . H284 H 0.2013 0.5694 0.0013 0.049 Uiso 1 1 calc R . . C285 C 0.15372(16) 0.7078(4) -0.02145(16) 0.0359(11) Uani 1 1 d . . . N291 N 0.07149(13) 0.7273(3) -0.05922(14) 0.0373(9) Uani 1 1 d . . . C292 C 0.11065(16) 0.6616(4) -0.05438(16) 0.0356(11) Uani 1 1 d . . . C293 C 0.10966(18) 0.5537(4) -0.07878(18) 0.0439(12) Uani 1 1 d . . . H293 H 0.1375 0.5084 -0.0748 0.053 Uiso 1 1 calc R . . C294 C 0.0685(2) 0.5127(4) -0.10861(19) 0.0538(14) Uani 1 1 d . . . H294 H 0.0675 0.4394 -0.1256 0.065 Uiso 1 1 calc R . . C295 C 0.0286(2) 0.5799(4) -0.1135(2) 0.0555(14) Uani 1 1 d . . . H295 H -0.0005 0.5531 -0.1335 0.067 Uiso 1 1 calc R . . C296 C 0.03154(18) 0.6858(4) -0.08901(18) 0.0454(12) Uani 1 1 d . . . H296 H 0.0040 0.7323 -0.0933 0.054 Uiso 1 1 calc R . . B10 B 0.4291(2) 0.2340(4) 0.2652(2) 0.0373(13) Uani 1 1 d . . . F11 F 0.40955(9) 0.2608(2) 0.30962(10) 0.0418(6) Uani 1 1 d . . . F12 F 0.42930(12) 0.1173(2) 0.25846(13) 0.0689(9) Uani 1 1 d . . . F13 F 0.4072(2) 0.2898(4) 0.22240(14) 0.146(2) Uani 1 1 d . . . F14 F 0.47583(14) 0.2679(3) 0.27514(17) 0.1018(14) Uani 1 1 d . . . B20 B 0.2600(3) 0.2111(5) 0.4872(3) 0.0587(18) Uani 1 1 d . . . F21 F 0.30105(12) 0.1834(3) 0.47102(14) 0.0767(10) Uani 1 1 d . . . F22 F 0.25541(16) 0.1684(6) 0.53346(19) 0.161(2) Uani 1 1 d . . . F23 F 0.22320(13) 0.1817(4) 0.44712(16) 0.0986(12) Uani 1 1 d . . . F24 F 0.2605(2) 0.3294(4) 0.4917(2) 0.148(2) Uani 1 1 d . . . B30 B 0.05672(18) 0.2663(5) 0.2589(2) 0.0384(13) Uani 1 1 d . . . F31 F 0.07570(12) 0.2288(3) 0.31047(13) 0.0729(10) Uani 1 1 d . . . F32 F 0.09067(11) 0.2744(3) 0.22822(15) 0.0760(10) Uani 1 1 d . . . F33 F 0.03481(8) 0.3718(2) 0.26161(10) 0.0454(7) Uani 1 1 d . . . F34 F 0.02338(9) 0.1835(2) 0.23623(11) 0.0529(7) Uani 1 1 d . . . N1 N 0.3314(3) 0.2922(8) 0.6218(3) 0.118(2) Uani 1 1 d D . . O2 O 0.3242(3) 0.3980(7) 0.6084(3) 0.170(3) Uani 1 1 d . A . O3 O 0.3570(4) 0.2590(15) 0.5902(6) 0.090(4) Uiso 0.406(17) 1 d PDU A 1 O3' O 0.3512(3) 0.2041(10) 0.6095(4) 0.089(3) Uiso 0.594(17) 1 d PDU A 2 C4 C 0.3100(3) 0.2595(9) 0.6690(5) 0.165(5) Uani 1 1 d . A . H4A H 0.2979 0.1802 0.6644 0.248 Uiso 1 1 calc R . . H4B H 0.2841 0.3126 0.6716 0.248 Uiso 1 1 calc R . . H4C H 0.3339 0.2643 0.7018 0.248 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0604(3) 0.0272(2) 0.0388(2) -0.00678(15) 0.00804(17) 0.00711(17) Ag2 0.0402(2) 0.02647(19) 0.0405(2) -0.00260(14) 0.01934(16) -0.00579(15) Ag3 0.0610(3) 0.0346(2) 0.0427(2) -0.00959(16) 0.01056(18) -0.00196(18) N111 0.039(2) 0.025(2) 0.035(2) 0.0020(16) 0.0062(17) 0.0061(17) C112 0.042(3) 0.019(2) 0.029(2) 0.0036(18) 0.0051(19) 0.0109(19) C113 0.045(3) 0.034(3) 0.038(3) -0.003(2) 0.009(2) 0.003(2) C114 0.053(3) 0.051(3) 0.041(3) -0.002(2) 0.017(2) 0.011(3) C115 0.047(3) 0.049(3) 0.047(3) 0.005(2) 0.018(2) 0.004(2) C116 0.038(3) 0.030(3) 0.047(3) 0.006(2) 0.005(2) 0.003(2) N121 0.041(2) 0.027(2) 0.0282(19) 0.0040(16) 0.0059(16) 0.0056(17) N122 0.043(2) 0.031(2) 0.030(2) 0.0052(17) 0.0104(17) 0.0045(18) C123 0.051(3) 0.025(3) 0.041(3) 0.003(2) 0.007(2) 0.001(2) C124 0.054(3) 0.023(2) 0.038(3) -0.003(2) 0.013(2) 0.001(2) C125 0.038(3) 0.024(2) 0.025(2) 0.0036(18) 0.0029(19) 0.009(2) C131 0.054(3) 0.038(3) 0.033(2) 0.007(2) 0.021(2) 0.008(2) C132 0.039(3) 0.034(3) 0.025(2) 0.0015(19) 0.019(2) 0.005(2) C133 0.028(2) 0.040(3) 0.029(2) 0.000(2) 0.0074(19) -0.002(2) C134 0.036(2) 0.031(3) 0.036(2) -0.003(2) 0.017(2) -0.004(2) C135 0.031(2) 0.031(2) 0.024(2) -0.0012(18) 0.0127(18) 0.0010(19) C136 0.038(3) 0.032(3) 0.026(2) -0.0069(19) 0.0109(19) -0.003(2) C137 0.047(3) 0.028(2) 0.032(2) -0.006(2) 0.016(2) 0.001(2) C138 0.037(2) 0.028(2) 0.031(2) -0.0024(19) 0.0133(19) 0.0011(19) N141 0.0300(19) 0.0244(19) 0.0244(18) 0.0001(15) 0.0071(15) 0.0010(15) N142 0.0318(19) 0.0242(19) 0.0293(19) 0.0001(15) 0.0057(15) 0.0001(15) C143 0.062(3) 0.021(2) 0.037(3) -0.003(2) 0.007(2) -0.010(2) C144 0.066(3) 0.031(3) 0.033(3) 0.005(2) 0.012(2) -0.021(2) C145 0.032(2) 0.025(2) 0.027(2) 0.0038(18) 0.0041(19) -0.0025(19) N151 0.0300(19) 0.029(2) 0.0221(18) 0.0018(15) 0.0056(15) 0.0010(16) C152 0.032(2) 0.031(2) 0.026(2) 0.0046(19) 0.0036(19) -0.002(2) C153 0.044(3) 0.049(3) 0.026(2) 0.000(2) 0.008(2) -0.013(2) C154 0.038(3) 0.073(4) 0.032(3) -0.001(3) 0.014(2) -0.017(3) C155 0.039(3) 0.060(3) 0.030(2) -0.005(2) 0.012(2) -0.003(2) C156 0.029(2) 0.039(3) 0.025(2) 0.004(2) 0.0017(18) 0.003(2) N161 0.037(2) 0.028(2) 0.0281(19) -0.0047(16) 0.0039(16) -0.0032(16) N162 0.051(2) 0.031(2) 0.032(2) -0.0094(17) 0.0081(18) -0.0053(18) C163 0.071(4) 0.040(3) 0.044(3) -0.020(2) 0.014(3) -0.007(3) C164 0.055(3) 0.049(3) 0.044(3) -0.015(2) 0.020(2) -0.002(3) C165 0.039(3) 0.035(3) 0.024(2) -0.0009(19) 0.0066(19) 0.002(2) C171 0.052(3) 0.032(3) 0.037(3) -0.003(2) 0.009(2) -0.014(2) C172 0.044(3) 0.025(2) 0.032(2) -0.0078(19) 0.005(2) -0.013(2) C173 0.052(3) 0.037(3) 0.026(2) -0.006(2) 0.007(2) -0.019(2) C174 0.046(3) 0.039(3) 0.042(3) -0.007(2) 0.015(2) -0.012(2) C175 0.040(3) 0.035(3) 0.045(3) 0.002(2) 0.010(2) -0.017(2) C176 0.055(3) 0.037(3) 0.033(3) 0.003(2) 0.011(2) -0.012(2) C177 0.048(3) 0.038(3) 0.032(3) -0.002(2) 0.015(2) -0.010(2) C178 0.038(3) 0.047(3) 0.055(3) 0.007(2) 0.010(2) -0.011(2) N181 0.041(2) 0.040(2) 0.036(2) 0.0000(18) 0.0111(18) -0.0072(18) N182 0.037(2) 0.043(2) 0.044(2) 0.006(2) 0.0111(18) -0.0025(18) C183 0.039(3) 0.057(3) 0.040(3) 0.009(2) 0.016(2) 0.014(2) C184 0.044(3) 0.042(3) 0.037(3) 0.000(2) 0.012(2) 0.008(2) C185 0.035(3) 0.035(3) 0.036(3) 0.000(2) 0.005(2) 0.004(2) N191 0.047(2) 0.037(2) 0.037(2) -0.0054(18) 0.0136(18) -0.0042(18) C192 0.035(3) 0.037(3) 0.035(3) -0.006(2) 0.006(2) -0.003(2) C193 0.054(3) 0.054(3) 0.050(3) -0.022(3) 0.018(3) -0.018(3) C194 0.070(4) 0.046(3) 0.076(4) -0.024(3) 0.022(3) -0.027(3) C195 0.067(4) 0.050(3) 0.063(4) 0.000(3) 0.022(3) -0.018(3) C196 0.057(3) 0.045(3) 0.044(3) -0.005(2) 0.021(2) -0.011(3) N211 0.042(2) 0.028(2) 0.034(2) -0.0038(16) 0.0102(17) -0.0039(17) C212 0.036(2) 0.021(2) 0.042(3) -0.009(2) 0.012(2) -0.010(2) C213 0.050(3) 0.027(3) 0.062(3) -0.010(2) 0.024(3) -0.007(2) C214 0.065(4) 0.044(3) 0.057(3) -0.020(3) 0.034(3) -0.015(3) C215 0.069(4) 0.047(3) 0.039(3) -0.009(2) 0.022(3) -0.009(3) C216 0.056(3) 0.032(3) 0.041(3) -0.005(2) 0.011(2) -0.004(2) N221 0.037(2) 0.027(2) 0.034(2) 0.0017(17) 0.0040(16) -0.0041(16) N222 0.037(2) 0.029(2) 0.036(2) 0.0036(17) 0.0043(17) -0.0050(17) C223 0.049(3) 0.027(3) 0.058(3) 0.010(2) 0.009(2) 0.004(2) C224 0.051(3) 0.027(3) 0.062(3) 0.002(2) 0.017(3) 0.004(2) C225 0.035(3) 0.021(2) 0.043(3) -0.002(2) 0.008(2) -0.0041(19) C231 0.040(3) 0.040(3) 0.031(2) 0.004(2) 0.008(2) -0.004(2) C232 0.036(2) 0.028(2) 0.029(2) 0.0074(19) 0.0054(19) 0.0023(19) C233 0.037(3) 0.040(3) 0.031(2) -0.008(2) 0.011(2) -0.002(2) C234 0.032(2) 0.041(3) 0.032(2) 0.000(2) 0.0144(19) 0.002(2) C235 0.029(2) 0.026(2) 0.029(2) 0.0056(18) 0.0055(18) 0.0075(18) C236 0.057(3) 0.042(3) 0.042(3) -0.009(2) 0.031(2) -0.004(2) C237 0.050(3) 0.049(3) 0.047(3) 0.001(2) 0.030(2) -0.007(2) C238 0.035(2) 0.031(2) 0.036(2) -0.004(2) 0.013(2) 0.006(2) N241 0.0291(19) 0.0224(19) 0.034(2) 0.0028(15) 0.0052(16) 0.0016(16) N242 0.030(2) 0.0225(19) 0.036(2) 0.0004(16) 0.0063(16) 0.0030(16) C243 0.043(3) 0.026(3) 0.052(3) 0.009(2) 0.006(2) 0.010(2) C244 0.050(3) 0.028(3) 0.054(3) 0.016(2) 0.014(2) 0.001(2) C245 0.039(3) 0.020(2) 0.029(2) -0.0003(18) 0.0051(19) -0.0039(19) N251 0.0265(19) 0.0227(19) 0.0279(18) -0.0013(15) 0.0073(14) -0.0028(15) C252 0.030(2) 0.029(2) 0.025(2) -0.0016(18) 0.0071(18) -0.0071(19) C253 0.041(3) 0.037(3) 0.037(3) 0.003(2) 0.007(2) -0.009(2) C254 0.037(3) 0.048(3) 0.038(3) 0.006(2) 0.012(2) -0.015(2) C255 0.025(2) 0.049(3) 0.035(2) -0.003(2) 0.0083(19) -0.005(2) C256 0.028(2) 0.033(2) 0.023(2) -0.0074(18) 0.0054(18) -0.0036(19) N261 0.0279(19) 0.028(2) 0.034(2) 0.0020(16) 0.0076(15) 0.0046(16) N262 0.037(2) 0.030(2) 0.031(2) 0.0000(16) 0.0075(16) 0.0082(17) C263 0.034(3) 0.047(3) 0.039(3) -0.003(2) 0.005(2) 0.015(2) C264 0.028(2) 0.045(3) 0.044(3) -0.006(2) 0.002(2) 0.004(2) C265 0.028(2) 0.038(3) 0.024(2) -0.0045(19) 0.0055(18) 0.004(2) C271 0.047(3) 0.026(2) 0.040(3) 0.001(2) 0.009(2) 0.008(2) C272 0.039(3) 0.028(3) 0.034(2) 0.003(2) 0.006(2) 0.006(2) C273 0.045(3) 0.037(3) 0.041(3) 0.002(2) 0.014(2) -0.009(2) C274 0.048(3) 0.038(3) 0.041(3) -0.010(2) 0.014(2) -0.012(2) C275 0.039(3) 0.041(3) 0.032(2) -0.001(2) 0.004(2) -0.007(2) C276 0.119(5) 0.053(4) 0.048(3) -0.006(3) 0.032(3) -0.041(4) C277 0.127(5) 0.039(3) 0.050(3) -0.016(3) 0.037(3) -0.032(3) C278 0.048(3) 0.053(3) 0.040(3) -0.008(2) 0.013(2) -0.023(2) N281 0.043(2) 0.042(2) 0.032(2) -0.0030(18) 0.0094(18) -0.0081(18) N282 0.038(2) 0.049(3) 0.033(2) -0.0051(19) 0.0114(18) -0.012(2) C283 0.039(3) 0.063(4) 0.035(3) 0.003(2) 0.018(2) -0.003(3) C284 0.047(3) 0.042(3) 0.038(3) 0.001(2) 0.020(2) 0.000(2) C285 0.045(3) 0.042(3) 0.024(2) 0.000(2) 0.016(2) -0.003(2) N291 0.044(2) 0.033(2) 0.035(2) -0.0015(17) 0.0051(18) -0.0056(19) C292 0.050(3) 0.034(3) 0.025(2) 0.001(2) 0.011(2) -0.009(2) C293 0.060(3) 0.034(3) 0.040(3) -0.001(2) 0.017(2) -0.003(2) C294 0.084(4) 0.032(3) 0.044(3) -0.008(2) 0.009(3) -0.017(3) C295 0.065(4) 0.041(3) 0.054(3) -0.006(3) -0.005(3) -0.019(3) C296 0.051(3) 0.035(3) 0.046(3) 0.002(2) -0.002(2) -0.008(2) B10 0.049(3) 0.031(3) 0.034(3) 0.000(2) 0.011(3) 0.000(3) F11 0.0497(16) 0.0404(15) 0.0395(15) -0.0009(12) 0.0191(12) 0.0043(12) F12 0.106(3) 0.0375(18) 0.075(2) -0.0157(15) 0.0458(19) -0.0114(16) F13 0.228(6) 0.167(5) 0.049(2) 0.037(2) 0.037(3) 0.134(4) F14 0.094(3) 0.112(3) 0.119(3) -0.059(3) 0.071(2) -0.044(2) B20 0.097(6) 0.041(4) 0.044(4) 0.004(3) 0.028(4) 0.012(4) F21 0.081(2) 0.073(2) 0.083(2) -0.0183(19) 0.033(2) -0.0067(19) F22 0.116(4) 0.261(7) 0.114(4) 0.116(4) 0.044(3) 0.004(4) F23 0.084(3) 0.122(3) 0.093(3) -0.033(3) 0.025(2) -0.003(2) F24 0.233(6) 0.064(3) 0.162(5) -0.031(3) 0.077(4) 0.028(3) B30 0.034(3) 0.032(3) 0.051(3) -0.004(3) 0.012(3) 0.000(2) F31 0.089(2) 0.0490(19) 0.069(2) 0.0156(16) -0.0160(18) -0.0117(17) F32 0.063(2) 0.058(2) 0.123(3) 0.0022(19) 0.057(2) 0.0057(16) F33 0.0416(15) 0.0373(16) 0.0582(17) -0.0092(13) 0.0118(13) 0.0059(12) F34 0.0523(17) 0.0430(17) 0.0657(18) -0.0184(14) 0.0165(14) -0.0010(13) N1 0.104(5) 0.118(7) 0.125(6) 0.002(5) 0.000(5) -0.029(5) O2 0.207(8) 0.145(6) 0.156(6) 0.042(5) 0.031(5) -0.061(6) C4 0.115(8) 0.164(10) 0.222(12) 0.099(9) 0.046(8) -0.014(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N211 2.271(3) . ? Ag1 N111 2.289(3) . ? Ag1 N121 2.392(4) . ? Ag1 N221 2.412(3) . ? Ag2 N251 2.398(3) . ? Ag2 N141 2.416(3) . ? Ag2 N151 2.424(3) . ? Ag2 N241 2.560(3) . ? Ag2 N261 2.592(3) . ? Ag2 N161 2.594(3) . ? Ag3 N291 2.246(4) . ? Ag3 N191 2.293(4) . ? Ag3 N181 2.403(4) . ? Ag3 N281 2.493(4) . ? N111 C116 1.344(6) . ? N111 C112 1.346(5) . ? C112 C113 1.384(6) . ? C112 C125 1.465(6) . ? C113 C114 1.381(6) . ? C114 C115 1.370(7) . ? C115 C116 1.379(6) . ? N121 C125 1.335(5) . ? N121 N122 1.352(5) . ? N122 C123 1.350(5) . ? N122 C131 1.464(5) . ? C123 C124 1.373(6) . ? C124 C125 1.404(6) . ? C131 C132 1.511(6) . ? C132 C137 1.391(6) . ? C132 C133 1.397(6) . ? C133 C134 1.381(6) . ? C134 C135 1.393(6) . ? C135 C136 1.389(6) . ? C135 C138 1.507(6) . ? C136 C137 1.391(6) . ? C138 N142 1.469(5) . ? N141 C145 1.328(5) . ? N141 N142 1.347(4) . ? N142 C143 1.346(5) . ? C143 C144 1.371(6) . ? C144 C145 1.395(6) . ? C145 C152 1.466(6) . ? N151 C156 1.339(5) . ? N151 C152 1.350(5) . ? C152 C153 1.392(6) . ? C153 C154 1.370(6) . ? C154 C155 1.377(6) . ? C155 C156 1.393(6) . ? C156 C165 1.472(6) . ? N161 C165 1.332(5) . ? N161 N162 1.350(5) . ? N162 C163 1.351(6) . ? N162 C171 1.451(5) . ? C163 C164 1.361(7) . ? C164 C165 1.417(6) . ? C171 C172 1.516(6) . ? C172 C173 1.387(6) . ? C172 C177 1.391(6) . ? C173 C174 1.390(6) . ? C174 C175 1.384(6) . ? C175 C176 1.387(6) . ? C175 C178 1.507(7) . ? C176 C177 1.383(6) . ? C178 N182 1.457(6) . ? N181 C185 1.338(6) . ? N181 N182 1.350(5) . ? N182 C183 1.344(6) . ? C183 C184 1.374(7) . ? C184 C185 1.397(6) . ? C185 C192 1.469(6) . ? N191 C196 1.343(6) . ? N191 C192 1.347(5) . ? C192 C193 1.386(6) . ? C193 C194 1.370(7) . ? C194 C195 1.388(7) . ? C195 C196 1.376(7) . ? N211 C216 1.344(6) . ? N211 C212 1.351(5) . ? C212 C213 1.389(6) . ? C212 C225 1.475(6) . ? C213 C214 1.381(7) . ? C214 C215 1.381(7) . ? C215 C216 1.380(6) . ? N221 C225 1.332(5) . ? N221 N222 1.354(5) . ? N222 C223 1.352(6) . ? N222 C231 1.446(5) . ? C223 C224 1.360(7) . ? C224 C225 1.398(6) . ? C231 C232 1.522(6) . ? C232 C233 1.378(6) . ? C232 C237 1.384(6) . ? C233 C234 1.390(6) . ? C234 C235 1.367(6) . ? C235 C236 1.390(6) . ? C235 C238 1.508(6) . ? C236 C237 1.377(6) . ? C238 N242 1.457(5) . ? N241 C245 1.340(5) . ? N241 N242 1.342(4) . ? N242 C243 1.341(5) . ? C243 C244 1.368(6) . ? C244 C245 1.399(6) . ? C245 C252 1.474(6) . ? N251 C256 1.345(5) . ? N251 C252 1.357(5) . ? C252 C253 1.389(6) . ? C253 C254 1.377(6) . ? C254 C255 1.380(6) . ? C255 C256 1.384(6) . ? C256 C265 1.475(6) . ? N261 C265 1.331(5) . ? N261 N262 1.360(5) . ? N262 C263 1.340(5) . ? N262 C271 1.458(5) . ? C263 C264 1.358(6) . ? C264 C265 1.404(6) . ? C271 C272 1.517(6) . ? C272 C273 1.365(6) . ? C272 C277 1.373(7) . ? C273 C274 1.381(6) . ? C274 C275 1.376(6) . ? C275 C276 1.380(7) . ? C275 C278 1.507(6) . ? C276 C277 1.378(7) . ? C278 N282 1.458(6) . ? N281 C285 1.348(6) . ? N281 N282 1.348(5) . ? N282 C283 1.343(6) . ? C283 C284 1.365(6) . ? C284 C285 1.402(6) . ? C285 C292 1.465(6) . ? N291 C296 1.345(6) . ? N291 C292 1.351(6) . ? C292 C293 1.391(6) . ? C293 C294 1.370(7) . ? C294 C295 1.378(7) . ? C295 C296 1.369(7) . ? B10 F13 1.319(6) . ? B10 F12 1.360(6) . ? B10 F14 1.386(6) . ? B10 F11 1.390(6) . ? B20 F22 1.304(7) . ? B20 F21 1.368(7) . ? B20 F23 1.370(8) . ? B20 F24 1.372(7) . ? B30 F32 1.368(6) . ? B30 F33 1.382(6) . ? B30 F31 1.391(6) . ? B30 F34 1.404(6) . ? N1 O3' 1.236(10) . ? N1 O3 1.249(13) . ? N1 O2 1.277(9) . ? N1 C4 1.500(12) . ? 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 N111 166.45(13) . . ? N211 Ag1 N121 120.51(12) . . ? N111 Ag1 N121 72.42(12) . . ? N211 Ag1 N221 71.63(12) . . ? N111 Ag1 N221 106.77(12) . . ? N121 Ag1 N221 118.71(11) . . ? N251 Ag2 N141 124.63(11) . . ? N251 Ag2 N151 165.79(11) . . ? N141 Ag2 N151 68.11(11) . . ? N251 Ag2 N241 67.79(11) . . ? N141 Ag2 N241 115.79(10) . . ? N151 Ag2 N241 101.88(11) . . ? N251 Ag2 N261 67.07(11) . . ? N141 Ag2 N261 85.24(11) . . ? N151 Ag2 N261 123.75(11) . . ? N241 Ag2 N261 134.36(10) . . ? N251 Ag2 N161 101.62(11) . . ? N141 Ag2 N161 133.64(11) . . ? N151 Ag2 N161 65.58(11) . . ? N241 Ag2 N161 76.36(10) . . ? N261 Ag2 N161 119.21(10) . . ? N291 Ag3 N191 161.77(13) . . ? N291 Ag3 N181 125.94(13) . . ? N191 Ag3 N181 72.22(13) . . ? N291 Ag3 N281 71.63(13) . . ? N191 Ag3 N281 99.83(13) . . ? N181 Ag3 N281 125.67(12) . . ? C116 N111 C112 117.4(4) . . ? C116 N111 Ag1 124.0(3) . . ? C112 N111 Ag1 116.2(3) . . ? N111 C112 C113 122.1(4) . . ? N111 C112 C125 117.3(4) . . ? C113 C112 C125 120.6(4) . . ? C114 C113 C112 119.3(4) . . ? C115 C114 C113 119.1(4) . . ? C114 C115 C116 118.5(5) . . ? N111 C116 C115 123.5(4) . . ? C125 N121 N122 105.1(3) . . ? C125 N121 Ag1 112.3(3) . . ? N122 N121 Ag1 142.3(3) . . ? C123 N122 N121 111.9(3) . . ? C123 N122 C131 127.7(4) . . ? N121 N122 C131 119.7(4) . . ? N122 C123 C124 107.0(4) . . ? C123 C124 C125 105.0(4) . . ? N121 C125 C124 111.0(4) . . ? N121 C125 C112 120.0(4) . . ? C124 C125 C112 129.1(4) . . ? N122 C131 C132 111.0(3) . . ? C137 C132 C133 118.5(4) . . ? C137 C132 C131 120.4(4) . . ? C133 C132 C131 121.1(4) . . ? C134 C133 C132 120.9(4) . . ? C133 C134 C135 120.4(4) . . ? C136 C135 C134 119.1(4) . . ? C136 C135 C138 120.5(4) . . ? C134 C135 C138 120.5(4) . . ? C135 C136 C137 120.5(4) . . ? C136 C137 C132 120.7(4) . . ? N142 C138 C135 111.7(3) . . ? C145 N141 N142 105.5(3) . . ? C145 N141 Ag2 116.8(3) . . ? N142 N141 Ag2 134.5(2) . . ? C143 N142 N141 111.7(3) . . ? C143 N142 C138 128.6(3) . . ? N141 N142 C138 119.4(3) . . ? N142 C143 C144 106.8(4) . . ? C143 C144 C145 105.3(4) . . ? N141 C145 C144 110.7(4) . . ? N141 C145 C152 118.7(4) . . ? C144 C145 C152 130.5(4) . . ? C156 N151 C152 119.3(4) . . ? C156 N151 Ag2 121.9(3) . . ? C152 N151 Ag2 118.2(3) . . ? N151 C152 C153 121.3(4) . . ? N151 C152 C145 115.7(4) . . ? C153 C152 C145 122.9(4) . . ? C154 C153 C152 119.0(4) . . ? C153 C154 C155 119.9(4) . . ? C154 C155 C156 118.6(4) . . ? N151 C156 C155 121.8(4) . . ? N151 C156 C165 115.6(4) . . ? C155 C156 C165 122.6(4) . . ? C165 N161 N162 106.0(3) . . ? C165 N161 Ag2 112.8(3) . . ? N162 N161 Ag2 133.9(3) . . ? N161 N162 C163 111.2(4) . . ? N161 N162 C171 119.2(3) . . ? C163 N162 C171 129.5(4) . . ? N162 C163 C164 107.7(4) . . ? C163 C164 C165 105.0(4) . . ? N161 C165 C164 110.1(4) . . ? N161 C165 C156 119.6(4) . . ? C164 C165 C156 130.3(4) . . ? N162 C171 C172 111.9(4) . . ? C173 C172 C177 118.5(4) . . ? C173 C172 C171 120.3(4) . . ? C177 C172 C171 121.1(4) . . ? C172 C173 C174 120.5(4) . . ? C175 C174 C173 120.9(4) . . ? C174 C175 C176 118.3(5) . . ? C174 C175 C178 121.5(4) . . ? C176 C175 C178 120.1(4) . . ? C177 C176 C175 121.0(4) . . ? C176 C177 C172 120.6(4) . . ? N182 C178 C175 111.2(4) . . ? C185 N181 N182 105.1(4) . . ? C185 N181 Ag3 111.8(3) . . ? N182 N181 Ag3 141.8(3) . . ? C183 N182 N181 112.0(4) . . ? C183 N182 C178 127.0(4) . . ? N181 N182 C178 120.5(4) . . ? N182 C183 C184 107.0(4) . . ? C183 C184 C185 105.3(4) . . ? N181 C185 C184 110.7(4) . . ? N181 C185 C192 120.7(4) . . ? C184 C185 C192 128.6(4) . . ? C196 N191 C192 118.3(4) . . ? C196 N191 Ag3 124.1(3) . . ? C192 N191 Ag3 117.2(3) . . ? N191 C192 C193 121.3(4) . . ? N191 C192 C185 117.2(4) . . ? C193 C192 C185 121.5(4) . . ? C194 C193 C192 119.6(5) . . ? C193 C194 C195 119.7(5) . . ? C196 C195 C194 117.5(5) . . ? N191 C196 C195 123.6(5) . . ? C216 N211 C212 117.5(4) . . ? C216 N211 Ag1 123.8(3) . . ? C212 N211 Ag1 117.1(3) . . ? N211 C212 C213 122.1(4) . . ? N211 C212 C225 116.8(4) . . ? C213 C212 C225 121.0(4) . . ? C214 C213 C212 119.1(5) . . ? C213 C214 C215 119.4(5) . . ? C216 C215 C214 118.2(5) . . ? N211 C216 C215 123.6(5) . . ? C225 N221 N222 105.4(3) . . ? C225 N221 Ag1 111.9(3) . . ? N222 N221 Ag1 141.2(3) . . ? C223 N222 N221 110.9(4) . . ? C223 N222 C231 128.6(4) . . ? N221 N222 C231 120.3(3) . . ? N222 C223 C224 107.7(4) . . ? C223 C224 C225 105.1(4) . . ? N221 C225 C224 110.9(4) . . ? N221 C225 C212 119.6(4) . . ? C224 C225 C212 129.5(4) . . ? N222 C231 C232 114.1(3) . . ? C233 C232 C237 118.2(4) . . ? C233 C232 C231 123.5(4) . . ? C237 C232 C231 118.3(4) . . ? C232 C233 C234 120.8(4) . . ? C235 C234 C233 121.3(4) . . ? C234 C235 C236 117.7(4) . . ? C234 C235 C238 124.1(4) . . ? C236 C235 C238 118.2(4) . . ? C237 C236 C235 121.5(4) . . ? C236 C237 C232 120.5(4) . . ? N242 C238 C235 115.3(3) . . ? C245 N241 N242 105.2(3) . . ? C245 N241 Ag2 113.6(3) . . ? N242 N241 Ag2 139.9(2) . . ? C243 N242 N241 111.9(3) . . ? C243 N242 C238 127.2(4) . . ? N241 N242 C238 120.7(3) . . ? N242 C243 C244 107.4(4) . . ? C243 C244 C245 104.9(4) . . ? N241 C245 C244 110.6(4) . . ? N241 C245 C252 120.1(4) . . ? C244 C245 C252 129.3(4) . . ? C256 N251 C252 118.6(3) . . ? C256 N251 Ag2 120.4(3) . . ? C252 N251 Ag2 120.7(2) . . ? N251 C252 C253 121.9(4) . . ? N251 C252 C245 116.7(3) . . ? C253 C252 C245 121.4(4) . . ? C254 C253 C252 118.5(4) . . ? C253 C254 C255 120.1(4) . . ? C254 C255 C256 118.7(4) . . ? N251 C256 C255 122.2(4) . . ? N251 C256 C265 116.2(3) . . ? C255 C256 C265 121.6(4) . . ? C265 N261 N262 104.6(3) . . ? C265 N261 Ag2 110.2(3) . . ? N262 N261 Ag2 136.9(2) . . ? C263 N262 N261 111.7(4) . . ? C263 N262 C271 128.1(4) . . ? N261 N262 C271 119.5(3) . . ? N262 C263 C264 107.6(4) . . ? C263 C264 C265 105.1(4) . . ? N261 C265 C264 111.0(4) . . ? N261 C265 C256 120.4(4) . . ? C264 C265 C256 128.6(4) . . ? N262 C271 C272 112.4(4) . . ? C273 C272 C277 117.2(4) . . ? C273 C272 C271 123.5(4) . . ? C277 C272 C271 119.3(4) . . ? C272 C273 C274 121.5(4) . . ? C275 C274 C273 121.3(4) . . ? C274 C275 C276 117.1(4) . . ? C274 C275 C278 123.4(4) . . ? C276 C275 C278 119.5(4) . . ? C277 C276 C275 120.9(5) . . ? C272 C277 C276 121.8(5) . . ? N282 C278 C275 112.5(4) . . ? C285 N281 N282 105.0(4) . . ? C285 N281 Ag3 107.2(3) . . ? N282 N281 Ag3 138.6(3) . . ? C283 N282 N281 111.5(4) . . ? C283 N282 C278 128.4(4) . . ? N281 N282 C278 119.9(4) . . ? N282 C283 C284 108.1(4) . . ? C283 C284 C285 104.7(4) . . ? N281 C285 C284 110.6(4) . . ? N281 C285 C292 120.0(4) . . ? C284 C285 C292 129.4(4) . . ? C296 N291 C292 117.9(4) . . ? C296 N291 Ag3 123.4(3) . . ? C292 N291 Ag3 118.6(3) . . ? N291 C292 C293 121.1(4) . . ? N291 C292 C285 117.1(4) . . ? C293 C292 C285 121.7(4) . . ? C294 C293 C292 120.0(5) . . ? C293 C294 C295 118.8(5) . . ? C296 C295 C294 119.0(5) . . ? N291 C296 C295 123.2(5) . . ? F13 B10 F12 113.3(5) . . ? F13 B10 F14 108.2(5) . . ? F12 B10 F14 106.1(4) . . ? F13 B10 F11 110.8(4) . . ? F12 B10 F11 109.6(4) . . ? F14 B10 F11 108.7(4) . . ? F22 B20 F21 115.0(6) . . ? F22 B20 F23 112.3(6) . . ? F21 B20 F23 108.4(5) . . ? F22 B20 F24 107.7(6) . . ? F21 B20 F24 105.1(6) . . ? F23 B20 F24 107.7(6) . . ? F32 B30 F33 110.7(4) . . ? F32 B30 F31 111.1(4) . . ? F33 B30 F31 109.4(4) . . ? F32 B30 F34 108.9(4) . . ? F33 B30 F34 109.6(4) . . ? F31 B30 F34 107.1(4) . . ? O3' N1 O3 39.4(7) . . ? O3' N1 O2 141.5(11) . . ? O3 N1 O2 102.2(11) . . ? O3' N1 C4 106.0(9) . . ? O3 N1 C4 145.2(12) . . ? O2 N1 C4 112.4(9) . . ? 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 C116 -25.5(7) . . . . ? N121 Ag1 N111 C116 171.2(3) . . . . ? N221 Ag1 N111 C116 55.7(3) . . . . ? N211 Ag1 N111 C112 172.5(4) . . . . ? N121 Ag1 N111 C112 9.1(3) . . . . ? N221 Ag1 N111 C112 -106.4(3) . . . . ? C116 N111 C112 C113 -0.5(6) . . . . ? Ag1 N111 C112 C113 162.7(3) . . . . ? C116 N111 C112 C125 -178.8(3) . . . . ? Ag1 N111 C112 C125 -15.5(4) . . . . ? N111 C112 C113 C114 -0.1(6) . . . . ? C125 C112 C113 C114 178.1(4) . . . . ? C112 C113 C114 C115 0.8(7) . . . . ? C113 C114 C115 C116 -0.8(7) . . . . ? C112 N111 C116 C115 0.5(6) . . . . ? Ag1 N111 C116 C115 -161.4(3) . . . . ? C114 C115 C116 N111 0.2(7) . . . . ? N211 Ag1 N121 C125 -177.0(2) . . . . ? N111 Ag1 N121 C125 -1.5(3) . . . . ? N221 Ag1 N121 C125 98.4(3) . . . . ? N211 Ag1 N121 N122 -5.5(5) . . . . ? N111 Ag1 N121 N122 170.1(4) . . . . ? N221 Ag1 N121 N122 -90.0(4) . . . . ? C125 N121 N122 C123 -0.6(4) . . . . ? Ag1 N121 N122 C123 -172.5(3) . . . . ? C125 N121 N122 C131 -172.1(3) . . . . ? Ag1 N121 N122 C131 16.0(6) . . . . ? N121 N122 C123 C124 1.0(5) . . . . ? C131 N122 C123 C124 171.7(4) . . . . ? N122 C123 C124 C125 -1.0(5) . . . . ? N122 N121 C125 C124 0.0(4) . . . . ? Ag1 N121 C125 C124 174.6(3) . . . . ? N122 N121 C125 C112 179.4(3) . . . . ? Ag1 N121 C125 C112 -5.9(4) . . . . ? C123 C124 C125 N121 0.6(5) . . . . ? C123 C124 C125 C112 -178.8(4) . . . . ? N111 C112 C125 N121 14.7(5) . . . . ? C113 C112 C125 N121 -163.6(4) . . . . ? N111 C112 C125 C124 -166.0(4) . . . . ? C113 C112 C125 C124 15.7(6) . . . . ? C123 N122 C131 C132 -98.7(5) . . . . ? N121 N122 C131 C132 71.3(5) . . . . ? N122 C131 C132 C137 71.7(5) . . . . ? N122 C131 C132 C133 -106.7(4) . . . . ? C137 C132 C133 C134 -2.0(6) . . . . ? C131 C132 C133 C134 176.5(4) . . . . ? C132 C133 C134 C135 0.2(6) . . . . ? C133 C134 C135 C136 1.2(6) . . . . ? C133 C134 C135 C138 -178.6(4) . . . . ? C134 C135 C136 C137 -0.8(6) . . . . ? C138 C135 C136 C137 179.0(4) . . . . ? C135 C136 C137 C132 -1.0(6) . . . . ? C133 C132 C137 C136 2.4(6) . . . . ? C131 C132 C137 C136 -176.1(4) . . . . ? C136 C135 C138 N142 -98.4(4) . . . . ? C134 C135 C138 N142 81.4(4) . . . . ? N251 Ag2 N141 C145 -176.3(3) . . . . ? N151 Ag2 N141 C145 10.9(3) . . . . ? N241 Ag2 N141 C145 103.9(3) . . . . ? N261 Ag2 N141 C145 -118.5(3) . . . . ? N161 Ag2 N141 C145 8.2(3) . . . . ? N251 Ag2 N141 N142 -20.0(4) . . . . ? N151 Ag2 N141 N142 167.2(4) . . . . ? N241 Ag2 N141 N142 -99.8(3) . . . . ? N261 Ag2 N141 N142 37.8(3) . . . . ? N161 Ag2 N141 N142 164.5(3) . . . . ? C145 N141 N142 C143 -1.0(4) . . . . ? Ag2 N141 N142 C143 -159.1(3) . . . . ? C145 N141 N142 C138 -175.7(3) . . . . ? Ag2 N141 N142 C138 26.2(5) . . . . ? C135 C138 N142 C143 -104.1(5) . . . . ? C135 C138 N142 N141 69.6(4) . . . . ? N141 N142 C143 C144 0.9(5) . . . . ? C138 N142 C143 C144 175.0(4) . . . . ? N142 C143 C144 C145 -0.4(5) . . . . ? N142 N141 C145 C144 0.7(5) . . . . ? Ag2 N141 C145 C144 163.4(3) . . . . ? N142 N141 C145 C152 178.7(3) . . . . ? Ag2 N141 C145 C152 -18.5(5) . . . . ? C143 C144 C145 N141 -0.2(5) . . . . ? C143 C144 C145 C152 -177.9(4) . . . . ? N251 Ag2 N151 C156 13.8(6) . . . . ? N141 Ag2 N151 C156 169.0(3) . . . . ? N241 Ag2 N151 C156 55.8(3) . . . . ? N261 Ag2 N151 C156 -123.1(3) . . . . ? N161 Ag2 N151 C156 -13.1(3) . . . . ? N251 Ag2 N151 C152 -157.5(4) . . . . ? N141 Ag2 N151 C152 -2.2(3) . . . . ? N241 Ag2 N151 C152 -115.4(3) . . . . ? N261 Ag2 N151 C152 65.7(3) . . . . ? N161 Ag2 N151 C152 175.7(3) . . . . ? C156 N151 C152 C153 -0.6(6) . . . . ? Ag2 N151 C152 C153 170.9(3) . . . . ? C156 N151 C152 C145 -177.3(3) . . . . ? Ag2 N151 C152 C145 -5.8(4) . . . . ? N141 C145 C152 N151 16.4(5) . . . . ? C144 C145 C152 N151 -166.0(4) . . . . ? N141 C145 C152 C153 -160.3(4) . . . . ? C144 C145 C152 C153 17.3(7) . . . . ? N151 C152 C153 C154 0.0(6) . . . . ? C145 C152 C153 C154 176.4(4) . . . . ? C152 C153 C154 C155 0.2(7) . . . . ? C153 C154 C155 C156 0.2(7) . . . . ? C152 N151 C156 C155 1.0(6) . . . . ? Ag2 N151 C156 C155 -170.1(3) . . . . ? C152 N151 C156 C165 178.4(3) . . . . ? Ag2 N151 C156 C165 7.3(5) . . . . ? C154 C155 C156 N151 -0.8(7) . . . . ? C154 C155 C156 C165 -178.1(4) . . . . ? N251 Ag2 N161 C165 -155.7(3) . . . . ? N141 Ag2 N161 C165 20.5(3) . . . . ? N151 Ag2 N161 C165 17.8(3) . . . . ? N241 Ag2 N161 C165 -92.3(3) . . . . ? N261 Ag2 N161 C165 134.2(3) . . . . ? N251 Ag2 N161 N162 -10.7(4) . . . . ? N141 Ag2 N161 N162 165.6(3) . . . . ? N151 Ag2 N161 N162 162.8(4) . . . . ? N241 Ag2 N161 N162 52.8(4) . . . . ? N261 Ag2 N161 N162 -80.7(4) . . . . ? C165 N161 N162 C163 -1.6(5) . . . . ? Ag2 N161 N162 C163 -148.3(3) . . . . ? C165 N161 N162 C171 -177.8(4) . . . . ? Ag2 N161 N162 C171 35.5(5) . . . . ? N161 N162 C163 C164 1.3(6) . . . . ? C171 N162 C163 C164 177.0(4) . . . . ? N162 C163 C164 C165 -0.5(6) . . . . ? N162 N161 C165 C164 1.2(5) . . . . ? Ag2 N161 C165 C164 155.8(3) . . . . ? N162 N161 C165 C156 -176.8(4) . . . . ? Ag2 N161 C165 C156 -22.2(5) . . . . ? C163 C164 C165 N161 -0.5(5) . . . . ? C163 C164 C165 C156 177.3(4) . . . . ? N151 C156 C165 N161 11.5(6) . . . . ? C155 C156 C165 N161 -171.0(4) . . . . ? N151 C156 C165 C164 -166.1(4) . . . . ? C155 C156 C165 C164 11.3(7) . . . . ? N161 N162 C171 C172 67.4(5) . . . . ? C163 N162 C171 C172 -108.0(5) . . . . ? N162 C171 C172 C173 -144.5(4) . . . . ? N162 C171 C172 C177 36.4(5) . . . . ? C177 C172 C173 C174 -0.7(6) . . . . ? C171 C172 C173 C174 -179.8(4) . . . . ? C172 C173 C174 C175 1.4(6) . . . . ? C173 C174 C175 C176 -0.2(6) . . . . ? C173 C174 C175 C178 -177.8(4) . . . . ? C174 C175 C176 C177 -1.7(6) . . . . ? C178 C175 C176 C177 175.9(4) . . . . ? C175 C176 C177 C172 2.5(7) . . . . ? C173 C172 C177 C176 -1.3(6) . . . . ? C171 C172 C177 C176 177.8(4) . . . . ? C174 C175 C178 N182 96.9(5) . . . . ? C176 C175 C178 N182 -80.7(5) . . . . ? N291 Ag3 N181 C185 173.9(3) . . . . ? N191 Ag3 N181 C185 -8.0(3) . . . . ? N281 Ag3 N181 C185 81.5(3) . . . . ? N291 Ag3 N181 N182 9.4(5) . . . . ? N191 Ag3 N181 N182 -172.5(5) . . . . ? N281 Ag3 N181 N182 -83.0(5) . . . . ? C185 N181 N182 C183 -0.5(5) . . . . ? Ag3 N181 N182 C183 164.6(3) . . . . ? C185 N181 N182 C178 -172.5(4) . . . . ? Ag3 N181 N182 C178 -7.4(7) . . . . ? C175 C178 N182 C183 -87.7(5) . . . . ? C175 C178 N182 N181 83.0(5) . . . . ? N181 N182 C183 C184 0.7(5) . . . . ? C178 N182 C183 C184 172.0(4) . . . . ? N182 C183 C184 C185 -0.6(5) . . . . ? N182 N181 C185 C184 0.2(5) . . . . ? Ag3 N181 C185 C184 -170.0(3) . . . . ? N182 N181 C185 C192 179.0(4) . . . . ? Ag3 N181 C185 C192 8.9(5) . . . . ? C183 C184 C185 N181 0.3(5) . . . . ? C183 C184 C185 C192 -178.5(4) . . . . ? N291 Ag3 N191 C196 -6.0(7) . . . . ? N181 Ag3 N191 C196 178.7(4) . . . . ? N281 Ag3 N191 C196 54.3(4) . . . . ? N291 Ag3 N191 C192 -178.0(4) . . . . ? N181 Ag3 N191 C192 6.7(3) . . . . ? N281 Ag3 N191 C192 -117.8(3) . . . . ? C196 N191 C192 C193 1.3(7) . . . . ? Ag3 N191 C192 C193 173.8(4) . . . . ? C196 N191 C192 C185 -177.2(4) . . . . ? Ag3 N191 C192 C185 -4.7(5) . . . . ? N181 C185 C192 N191 -3.3(6) . . . . ? C184 C185 C192 N191 175.3(4) . . . . ? N181 C185 C192 C193 178.2(4) . . . . ? C184 C185 C192 C193 -3.2(7) . . . . ? N191 C192 C193 C194 0.6(8) . . . . ? C185 C192 C193 C194 179.1(5) . . . . ? C192 C193 C194 C195 -2.1(9) . . . . ? C193 C194 C195 C196 1.6(9) . . . . ? C192 N191 C196 C195 -1.8(7) . . . . ? Ag3 N191 C196 C195 -173.8(4) . . . . ? C194 C195 C196 N191 0.4(8) . . . . ? N111 Ag1 N211 C216 -94.1(6) . . . . ? N121 Ag1 N211 C216 67.4(4) . . . . ? N221 Ag1 N211 C216 -179.5(4) . . . . ? N111 Ag1 N211 C212 100.4(6) . . . . ? N121 Ag1 N211 C212 -98.1(3) . . . . ? N221 Ag1 N211 C212 15.0(3) . . . . ? C216 N211 C212 C213 -3.3(6) . . . . ? Ag1 N211 C212 C213 163.2(3) . . . . ? C216 N211 C212 C225 178.8(4) . . . . ? Ag1 N211 C212 C225 -14.8(5) . . . . ? N211 C212 C213 C214 2.6(7) . . . . ? C225 C212 C213 C214 -179.5(4) . . . . ? C212 C213 C214 C215 -0.1(7) . . . . ? C213 C214 C215 C216 -1.6(7) . . . . ? C212 N211 C216 C215 1.4(7) . . . . ? Ag1 N211 C216 C215 -164.0(4) . . . . ? C214 C215 C216 N211 1.0(7) . . . . ? N211 Ag1 N221 C225 -13.6(3) . . . . ? N111 Ag1 N221 C225 -179.5(3) . . . . ? N121 Ag1 N221 C225 101.8(3) . . . . ? N211 Ag1 N221 N222 -176.1(4) . . . . ? N111 Ag1 N221 N222 18.0(4) . . . . ? N121 Ag1 N221 N222 -60.8(4) . . . . ? C225 N221 N222 C223 -0.1(4) . . . . ? Ag1 N221 N222 C223 163.2(3) . . . . ? C225 N221 N222 C231 -175.5(4) . . . . ? Ag1 N221 N222 C231 -12.2(6) . . . . ? N221 N222 C223 C224 0.3(5) . . . . ? C231 N222 C223 C224 175.2(4) . . . . ? N222 C223 C224 C225 -0.4(5) . . . . ? N222 N221 C225 C224 -0.2(5) . . . . ? Ag1 N221 C225 C224 -169.0(3) . . . . ? N222 N221 C225 C212 -179.8(3) . . . . ? Ag1 N221 C225 C212 11.5(5) . . . . ? C223 C224 C225 N221 0.4(5) . . . . ? C223 C224 C225 C212 179.9(4) . . . . ? N211 C212 C225 N221 1.3(6) . . . . ? C213 C212 C225 N221 -176.6(4) . . . . ? N211 C212 C225 C224 -178.2(4) . . . . ? C213 C212 C225 C224 3.9(7) . . . . ? C223 N222 C231 C232 -101.8(5) . . . . ? N221 N222 C231 C232 72.7(5) . . . . ? N222 C231 C232 C233 3.1(6) . . . . ? N222 C231 C232 C237 -177.6(4) . . . . ? C237 C232 C233 C234 0.3(6) . . . . ? C231 C232 C233 C234 179.6(4) . . . . ? C232 C233 C234 C235 -0.8(7) . . . . ? C233 C234 C235 C236 1.1(6) . . . . ? C233 C234 C235 C238 -178.5(4) . . . . ? C234 C235 C236 C237 -1.1(7) . . . . ? C238 C235 C236 C237 178.5(4) . . . . ? C235 C236 C237 C232 0.7(7) . . . . ? C233 C232 C237 C236 -0.3(7) . . . . ? C231 C232 C237 C236 -179.6(4) . . . . ? C234 C235 C238 N242 -6.3(6) . . . . ? C236 C235 C238 N242 174.1(4) . . . . ? N251 Ag2 N241 C245 -6.1(3) . . . . ? N141 Ag2 N241 C245 112.8(3) . . . . ? N151 Ag2 N241 C245 -175.9(3) . . . . ? N261 Ag2 N241 C245 2.7(3) . . . . ? N161 Ag2 N241 C245 -115.0(3) . . . . ? N251 Ag2 N241 N242 -170.3(4) . . . . ? N141 Ag2 N241 N242 -51.3(4) . . . . ? N151 Ag2 N241 N242 19.9(4) . . . . ? N261 Ag2 N241 N242 -161.4(3) . . . . ? N161 Ag2 N241 N242 80.9(4) . . . . ? C245 N241 N242 C243 0.5(4) . . . . ? Ag2 N241 N242 C243 165.5(3) . . . . ? C245 N241 N242 C238 176.5(3) . . . . ? Ag2 N241 N242 C238 -18.5(6) . . . . ? C235 C238 N242 C243 -109.2(5) . . . . ? C235 C238 N242 N241 75.5(5) . . . . ? N241 N242 C243 C244 -0.6(5) . . . . ? C238 N242 C243 C244 -176.3(4) . . . . ? N242 C243 C244 C245 0.4(5) . . . . ? N242 N241 C245 C244 -0.3(5) . . . . ? Ag2 N241 C245 C244 -169.8(3) . . . . ? N242 N241 C245 C252 -178.7(3) . . . . ? Ag2 N241 C245 C252 11.8(4) . . . . ? C243 C244 C245 N241 -0.1(5) . . . . ? C243 C244 C245 C252 178.2(4) . . . . ? N141 Ag2 N251 C256 80.0(3) . . . . ? N151 Ag2 N251 C256 -128.2(4) . . . . ? N241 Ag2 N251 C256 -173.2(3) . . . . ? N261 Ag2 N251 C256 13.7(3) . . . . ? N161 Ag2 N251 C256 -103.3(3) . . . . ? N141 Ag2 N251 C252 -106.9(3) . . . . ? N151 Ag2 N251 C252 44.9(6) . . . . ? N241 Ag2 N251 C252 -0.1(3) . . . . ? N261 Ag2 N251 C252 -173.2(3) . . . . ? N161 Ag2 N251 C252 69.8(3) . . . . ? C256 N251 C252 C253 0.7(6) . . . . ? Ag2 N251 C252 C253 -172.5(3) . . . . ? C256 N251 C252 C245 179.2(3) . . . . ? Ag2 N251 C252 C245 5.9(4) . . . . ? N241 C245 C252 N251 -12.3(5) . . . . ? C244 C245 C252 N251 169.6(4) . . . . ? N241 C245 C252 C253 166.1(4) . . . . ? C244 C245 C252 C253 -11.9(7) . . . . ? N251 C252 C253 C254 -0.1(6) . . . . ? C245 C252 C253 C254 -178.4(4) . . . . ? C252 C253 C254 C255 -0.5(6) . . . . ? C253 C254 C255 C256 0.5(6) . . . . ? C252 N251 C256 C255 -0.8(6) . . . . ? Ag2 N251 C256 C255 172.4(3) . . . . ? C252 N251 C256 C265 -179.4(3) . . . . ? Ag2 N251 C256 C265 -6.1(4) . . . . ? C254 C255 C256 N251 0.2(6) . . . . ? C254 C255 C256 C265 178.7(4) . . . . ? N251 Ag2 N261 C265 -20.0(2) . . . . ? N141 Ag2 N261 C265 -150.9(3) . . . . ? N151 Ag2 N261 C265 149.5(2) . . . . ? N241 Ag2 N261 C265 -28.9(3) . . . . ? N161 Ag2 N261 C265 70.8(3) . . . . ? N251 Ag2 N261 N262 -161.8(4) . . . . ? N141 Ag2 N261 N262 67.3(4) . . . . ? N151 Ag2 N261 N262 7.7(4) . . . . ? N241 Ag2 N261 N262 -170.7(3) . . . . ? N161 Ag2 N261 N262 -71.0(4) . . . . ? C265 N261 N262 C263 -0.9(4) . . . . ? Ag2 N261 N262 C263 142.2(3) . . . . ? C265 N261 N262 C271 -172.5(3) . . . . ? Ag2 N261 N262 C271 -29.4(5) . . . . ? N261 N262 C263 C264 0.9(5) . . . . ? C271 N262 C263 C264 171.5(4) . . . . ? N262 C263 C264 C265 -0.4(5) . . . . ? N262 N261 C265 C264 0.6(4) . . . . ? Ag2 N261 C265 C264 -153.4(3) . . . . ? N262 N261 C265 C256 -179.7(3) . . . . ? Ag2 N261 C265 C256 26.2(4) . . . . ? C263 C264 C265 N261 -0.2(5) . . . . ? C263 C264 C265 C256 -179.7(4) . . . . ? N251 C256 C265 N261 -15.6(5) . . . . ? C255 C256 C265 N261 165.8(4) . . . . ? N251 C256 C265 C264 163.9(4) . . . . ? C255 C256 C265 C264 -14.6(6) . . . . ? C263 N262 C271 C272 -92.6(5) . . . . ? N261 N262 C271 C272 77.4(5) . . . . ? N262 C271 C272 C273 -5.5(6) . . . . ? N262 C271 C272 C277 175.1(5) . . . . ? C277 C272 C273 C274 3.4(7) . . . . ? C271 C272 C273 C274 -176.0(4) . . . . ? C272 C273 C274 C275 -1.1(7) . . . . ? C273 C274 C275 C276 -2.0(7) . . . . ? C273 C274 C275 C278 176.8(4) . . . . ? C274 C275 C276 C277 2.8(9) . . . . ? C278 C275 C276 C277 -176.1(6) . . . . ? C273 C272 C277 C276 -2.6(9) . . . . ? C271 C272 C277 C276 176.8(5) . . . . ? C275 C276 C277 C272 -0.5(10) . . . . ? C274 C275 C278 N282 3.1(7) . . . . ? C276 C275 C278 N282 -178.1(5) . . . . ? N291 Ag3 N281 C285 -18.7(3) . . . . ? N191 Ag3 N281 C285 177.9(3) . . . . ? N181 Ag3 N281 C285 102.8(3) . . . . ? N291 Ag3 N281 N282 -158.4(4) . . . . ? N191 Ag3 N281 N282 38.2(4) . . . . ? N181 Ag3 N281 N282 -36.9(5) . . . . ? C285 N281 N282 C283 -0.5(5) . . . . ? Ag3 N281 N282 C283 139.7(4) . . . . ? C285 N281 N282 C278 -175.7(4) . . . . ? Ag3 N281 N282 C278 -35.5(6) . . . . ? C275 C278 N282 C283 -89.4(5) . . . . ? C275 C278 N282 N281 84.9(5) . . . . ? N281 N282 C283 C284 0.4(5) . . . . ? C278 N282 C283 C284 175.1(4) . . . . ? N282 C283 C284 C285 -0.1(5) . . . . ? N282 N281 C285 C284 0.4(4) . . . . ? Ag3 N281 C285 C284 -153.3(3) . . . . ? N282 N281 C285 C292 179.5(3) . . . . ? Ag3 N281 C285 C292 25.8(4) . . . . ? C283 C284 C285 N281 -0.2(5) . . . . ? C283 C284 C285 C292 -179.2(4) . . . . ? N191 Ag3 N291 C296 -107.1(5) . . . . ? N181 Ag3 N291 C296 67.4(4) . . . . ? N281 Ag3 N291 C296 -171.4(4) . . . . ? N191 Ag3 N291 C292 75.2(5) . . . . ? N181 Ag3 N291 C292 -110.3(3) . . . . ? N281 Ag3 N291 C292 10.9(3) . . . . ? C296 N291 C292 C293 -0.9(6) . . . . ? Ag3 N291 C292 C293 177.0(3) . . . . ? C296 N291 C292 C285 -179.6(4) . . . . ? Ag3 N291 C292 C285 -1.7(5) . . . . ? N281 C285 C292 N291 -18.7(6) . . . . ? C284 C285 C292 N291 160.2(4) . . . . ? N281 C285 C292 C293 162.6(4) . . . . ? C284 C285 C292 C293 -18.5(7) . . . . ? N291 C292 C293 C294 0.4(7) . . . . ? C285 C292 C293 C294 179.0(4) . . . . ? C292 C293 C294 C295 -0.4(7) . . . . ? C293 C294 C295 C296 0.9(8) . . . . ? C292 N291 C296 C295 1.4(7) . . . . ? Ag3 N291 C296 C295 -176.3(4) . . . . ? C294 C295 C296 N291 -1.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.954 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.073 #===END data_Ag4 _database_code_depnum_ccdc_archive 'CCDC 265436' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H79 Ag4 B4 F16 N25' _chemical_formula_weight 2313.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 19.066(3) _cell_length_b 28.822(4) _cell_length_c 19.716(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.093(2) _cell_angle_gamma 90.00 _cell_volume 9812(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4632 _exptl_absorpt_coefficient_mu 0.876 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8107 _exptl_absorpt_correction_T_max 0.9175 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82310 _diffrn_reflns_av_R_equivalents 0.1060 _diffrn_reflns_av_sigmaI/netI 0.1563 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.53 _reflns_number_total 22151 _reflns_number_gt 9401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22151 _refine_ls_number_parameters 522 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.2475 _refine_ls_R_factor_gt 0.1622 _refine_ls_wR_factor_ref 0.5148 _refine_ls_wR_factor_gt 0.4759 _refine_ls_goodness_of_fit_ref 1.481 _refine_ls_restrained_S_all 1.478 _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 0.76287(6) 0.09088(4) 0.32662(7) 0.0372(4) Uani 1 1 d U . . Ag2 Ag 0.73741(6) 0.09099(4) 0.17324(7) 0.0375(4) Uani 1 1 d U . . Ag3 Ag 0.82490(8) 0.11360(4) 0.68727(7) 0.0418(4) Uani 1 1 d . . . Ag4 Ag 0.67574(13) 0.11340(10) -0.18680(12) 0.1187(10) Uani 1 1 d . . . N111 N 0.7488(4) 0.1773(3) 0.6373(4) 0.031(3) Uani 1 1 d G . . C112 C 0.7720(4) 0.2064(3) 0.5944(4) 0.025(3) Uiso 1 1 d G . . C113 C 0.7222(4) 0.2405(3) 0.5500(4) 0.023(3) Uiso 1 1 d G . . H11A H 0.7381 0.2604 0.5207 0.028 Uiso 1 1 calc R . . C114 C 0.6491(4) 0.2456(3) 0.5486(5) 0.033(3) Uiso 1 1 d G . . H11B H 0.6150 0.2690 0.5182 0.039 Uiso 1 1 calc R . . C115 C 0.6258(4) 0.2166(3) 0.5915(5) 0.039(4) Uiso 1 1 d G . . H11C H 0.5759 0.2201 0.5905 0.047 Uiso 1 1 calc R . . C116 C 0.6757(5) 0.1824(3) 0.6359(5) 0.041(4) Uiso 1 1 d G . . H11D H 0.6598 0.1626 0.6652 0.050 Uiso 1 1 calc R . . N121 N 0.8835(5) 0.1544(2) 0.6237(4) 0.0272(19) Uani 1 1 d GU . . N122 N 0.9517(4) 0.1541(2) 0.6114(4) 0.0270(19) Uani 1 1 d GU . . C123 C 0.9542(4) 0.1962(3) 0.5751(5) 0.023(3) Uiso 1 1 d G . . H12A H 0.9935 0.2052 0.5602 0.028 Uiso 1 1 calc R . . C124 C 0.8875(5) 0.2226(2) 0.5649(5) 0.023(3) Uiso 1 1 d G . . H12B H 0.8744 0.2522 0.5420 0.028 Uiso 1 1 calc R . . C125 C 0.8439(4) 0.1967(3) 0.5949(5) 0.022(3) Uiso 1 1 d G . . C131 C 0.9967(7) 0.1139(4) 0.6277(7) 0.024(3) Uiso 1 1 d . . . H13A H 1.0037 0.1020 0.6773 0.029 Uiso 1 1 calc R . . H13B H 1.0485 0.1215 0.6305 0.029 Uiso 1 1 calc R . . C132 C 0.9592(4) 0.0754(2) 0.5679(4) 0.013(2) Uiso 1 1 d G . . C133 C 0.9156(5) 0.0401(3) 0.5791(3) 0.026(3) Uiso 1 1 d G . . H13C H 0.9108 0.0382 0.6251 0.031 Uiso 1 1 calc R . . C134 C 0.8791(4) 0.0075(2) 0.5231(4) 0.026(3) Uiso 1 1 d G . . H13D H 0.8493 -0.0166 0.5308 0.031 Uiso 1 1 calc R . . C135 C 0.8861(4) 0.0103(2) 0.4559(4) 0.022(3) Uiso 1 1 d G . . C136 C 0.9297(5) 0.0457(3) 0.4447(3) 0.022(3) Uiso 1 1 d G . . H13E H 0.9345 0.0476 0.3988 0.027 Uiso 1 1 calc R . . C137 C 0.9662(4) 0.0782(2) 0.5007(4) 0.025(3) Uiso 1 1 d G . . H13F H 0.9960 0.1024 0.4931 0.030 Uiso 1 1 calc R . . C138 C 0.8465(8) -0.0240(5) 0.3973(8) 0.032(3) Uiso 1 1 d . . . H13G H 0.8631 -0.0197 0.3565 0.039 Uiso 1 1 calc R . . H13H H 0.8627 -0.0554 0.4184 0.039 Uiso 1 1 calc R . . N141 N 0.7243(5) 0.0199(3) 0.3292(5) 0.039(2) Uani 1 1 d GU . . N142 N 0.7632(4) -0.0210(3) 0.3663(5) 0.039(2) Uani 1 1 d GU . . C143 C 0.7063(6) -0.0540(3) 0.3628(7) 0.053(4) Uiso 1 1 d G . . H14A H 0.7161 -0.0844 0.3831 0.063 Uiso 1 1 calc R . . C144 C 0.6323(5) -0.0334(4) 0.3235(8) 0.075(6) Uiso 1 1 d G . . H14B H 0.5838 -0.0477 0.3129 0.090 Uiso 1 1 calc R . . C145 C 0.6434(5) 0.0123(4) 0.3027(6) 0.044(4) Uiso 1 1 d G . . N151 N 0.6219(5) 0.0852(4) 0.2426(5) 0.047(4) Uani 1 1 d G . . C152 C 0.5936(7) 0.0445(4) 0.2596(7) 0.074(6) Uiso 1 1 d G . . C153 C 0.5142(8) 0.0379(4) 0.2336(9) 0.080(7) Uiso 1 1 d G . . H15A H 0.4948 0.0101 0.2451 0.096 Uiso 1 1 calc R . . C154 C 0.4631(5) 0.0720(6) 0.1905(9) 0.095(8) Uiso 1 1 d G . . H15B H 0.4089 0.0675 0.1727 0.115 Uiso 1 1 calc R . . C155 C 0.4915(7) 0.1127(5) 0.1736(8) 0.103(9) Uiso 1 1 d G . . H15C H 0.4566 0.1360 0.1442 0.123 Uiso 1 1 calc R . . C156 C 0.5709(7) 0.1193(4) 0.1996(7) 0.065(5) Uiso 1 1 d G . . N161 N 0.6720(6) 0.1538(3) 0.1718(6) 0.047(3) Uani 1 1 d GU . . N162 N 0.6875(5) 0.1977(4) 0.1486(6) 0.048(3) Uani 1 1 d GU . . C163 C 0.6235(7) 0.2272(3) 0.1359(7) 0.062(5) Uiso 1 1 d G . . H16A H 0.6183 0.2586 0.1199 0.074 Uiso 1 1 calc R . . C164 C 0.5684(5) 0.2014(4) 0.1513(9) 0.083(7) Uiso 1 1 d G . . H16B H 0.5199 0.2126 0.1474 0.100 Uiso 1 1 calc R . . C165 C 0.5984(6) 0.1560(4) 0.1735(7) 0.055(5) Uiso 1 1 d G . . C171 C 0.7604(9) 0.2094(6) 0.1439(9) 0.043(4) Uiso 1 1 d . . . H17A H 0.8018 0.2149 0.1947 0.052 Uiso 1 1 calc R . . H17B H 0.7538 0.2380 0.1140 0.052 Uiso 1 1 calc R . . C172 C 0.7829(5) 0.1686(3) 0.1066(6) 0.039(4) Uiso 1 1 d G . . C173 C 0.8615(5) 0.1676(3) 0.1238(5) 0.044(4) Uiso 1 1 d G . . H17C H 0.8958 0.1889 0.1591 0.053 Uiso 1 1 calc R . . C174 C 0.8900(4) 0.1354(3) 0.0893(5) 0.037(3) Uiso 1 1 d G . . H17D H 0.9438 0.1347 0.1010 0.044 Uiso 1 1 calc R . . C175 C 0.8399(5) 0.1043(3) 0.0376(5) 0.032(3) Uiso 1 1 d G . . C176 C 0.7613(5) 0.1053(3) 0.0204(5) 0.050(4) Uiso 1 1 d G . . H17E H 0.7270 0.0840 -0.0149 0.060 Uiso 1 1 calc R . . C177 C 0.7328(4) 0.1375(4) 0.0549(6) 0.048(4) Uiso 1 1 d G . . H17F H 0.6790 0.1382 0.0432 0.058 Uiso 1 1 calc R . . C178 C 0.8749(9) 0.0715(6) -0.0015(9) 0.044(4) Uiso 1 1 d . . . H17G H 0.8930 0.0901 -0.0332 0.053 Uiso 1 1 calc R . . H17H H 0.9206 0.0558 0.0370 0.053 Uiso 1 1 calc R . . N181 N 0.7706(6) 0.0498(3) -0.1192(5) 0.054(3) Uani 1 1 d GU . . N182 N 0.8242(5) 0.0387(3) -0.0451(5) 0.053(3) Uani 1 1 d GU . . C183 C 0.8157(6) -0.0091(4) -0.0329(5) 0.048(4) Uiso 1 1 d G . . H18A H 0.8443 -0.0259 0.0119 0.057 Uiso 1 1 calc R . . C184 C 0.7569(7) -0.0276(3) -0.0996(7) 0.061(5) Uiso 1 1 d G . . H18B H 0.7393 -0.0588 -0.1072 0.074 Uiso 1 1 calc R . . C185 C 0.7290(6) 0.0089(4) -0.1529(5) 0.065(5) Uiso 1 1 d G . . N191 N 0.6398(10) 0.0513(6) -0.2559(9) 0.113(9) Uani 1 1 d G . . C192 C 0.6749(9) 0.0097(7) -0.2234(8) 0.088(7) Uiso 1 1 d G . . C193 C 0.6548(13) -0.0311(5) -0.2650(14) 0.126(11) Uiso 1 1 d G . . H19A H 0.6787 -0.0595 -0.2428 0.152 Uiso 1 1 calc R . . C194 C 0.5996(14) -0.0302(8) -0.3389(13) 0.25(2) Uiso 1 1 d G . . H19B H 0.5859 -0.0581 -0.3673 0.301 Uiso 1 1 calc R . . C195 C 0.5646(12) 0.0114(10) -0.3714(8) 0.203(19) Uiso 1 1 d G . . H19C H 0.5269 0.0120 -0.4219 0.244 Uiso 1 1 calc R . . C196 C 0.5847(11) 0.0522(8) -0.3298(10) 0.196(18) Uiso 1 1 d G . . H19D H 0.5607 0.0806 -0.3520 0.235 Uiso 1 1 calc R . . N211 N 0.8623(4) 0.05055(19) 0.7567(3) 0.019(2) Uani 1 1 d G . . C212 C 0.8266(4) 0.0088(2) 0.7258(3) 0.015(2) Uiso 1 1 d G . . C213 C 0.8465(4) -0.03149(19) 0.7686(4) 0.020(3) Uiso 1 1 d G . . H21A H 0.8221 -0.0600 0.7475 0.024 Uiso 1 1 calc R . . C214 C 0.9023(5) -0.0300(2) 0.8423(4) 0.029(3) Uiso 1 1 d G . . H21B H 0.9160 -0.0576 0.8715 0.035 Uiso 1 1 calc R . . C215 C 0.9381(4) 0.0117(3) 0.8732(3) 0.023(3) Uiso 1 1 d G . . H21C H 0.9762 0.0127 0.9235 0.027 Uiso 1 1 calc R . . C216 C 0.9181(4) 0.0520(2) 0.8304(4) 0.016(2) Uiso 1 1 d G . . H21D H 0.9425 0.0805 0.8515 0.019 Uiso 1 1 calc R . . N221 N 0.7322(5) 0.0496(2) 0.6189(5) 0.041(2) Uani 1 1 d GU . . N222 N 0.6776(5) 0.0385(3) 0.5451(4) 0.042(2) Uani 1 1 d GU . . C223 C 0.6833(6) -0.0097(3) 0.5338(4) 0.059(5) Uiso 1 1 d G . . H22A H 0.6535 -0.0265 0.4894 0.071 Uiso 1 1 calc R . . C224 C 0.7415(6) -0.0285(2) 0.6006(5) 0.037(3) Uiso 1 1 d G . . H22B H 0.7574 -0.0600 0.6086 0.044 Uiso 1 1 calc R . . C225 C 0.7717(5) 0.0082(3) 0.6531(4) 0.024(3) Uiso 1 1 d G . . C231 C 0.6264(12) 0.0720(7) 0.5009(12) 0.069(6) Uiso 1 1 d . . . H23A H 0.6077 0.0901 0.5327 0.083 Uiso 1 1 calc R . . H23B H 0.5810 0.0561 0.4622 0.083 Uiso 1 1 calc R . . C232 C 0.6582(5) 0.1053(3) 0.4624(6) 0.053(4) Uiso 1 1 d G . . C233 C 0.6074(4) 0.1365(4) 0.4113(6) 0.051(4) Uiso 1 1 d G . . H23C H 0.5538 0.1357 0.4003 0.061 Uiso 1 1 calc R . . C234 C 0.6349(5) 0.1688(3) 0.3761(5) 0.045(4) Uiso 1 1 d G . . H23D H 0.6002 0.1901 0.3412 0.054 Uiso 1 1 calc R . . C235 C 0.7133(5) 0.1699(3) 0.3921(5) 0.040(4) Uiso 1 1 d G . . C236 C 0.7641(4) 0.1388(3) 0.4432(5) 0.025(3) Uiso 1 1 d G . . H23E H 0.8156 0.1523 0.4763 0.030 Uiso 1 1 calc R . . C237 C 0.7365(5) 0.1064(3) 0.4783(5) 0.033(3) Uiso 1 1 d G . . H23F H 0.7712 0.0851 0.5133 0.039 Uiso 1 1 calc R . . C238 C 0.7465(9) 0.2079(6) 0.3552(9) 0.040(4) Uiso 1 1 d . . . H23G H 0.7074 0.2138 0.3035 0.048 Uiso 1 1 calc R . . H23H H 0.7538 0.2372 0.3836 0.048 Uiso 1 1 calc R . . N241 N 0.8266(4) 0.1533(2) 0.3265(5) 0.029(2) Uani 1 1 d GU . . N242 N 0.8131(4) 0.1967(3) 0.3529(5) 0.029(2) Uani 1 1 d GU . . C243 C 0.8768(5) 0.2262(2) 0.3642(5) 0.033(3) Uiso 1 1 d G . . H24A H 0.8830 0.2573 0.3816 0.040 Uiso 1 1 calc R . . C244 C 0.9296(4) 0.2010(3) 0.3447(5) 0.028(3) Uiso 1 1 d G . . H24B H 0.9773 0.2123 0.3469 0.034 Uiso 1 1 calc R . . C245 C 0.8986(4) 0.1559(3) 0.3215(5) 0.018(2) Uiso 1 1 d G . . N251 N 0.8793(3) 0.0845(3) 0.2572(4) 0.027(3) Uani 1 1 d G . . C252 C 0.9294(4) 0.1183(2) 0.3025(4) 0.019(2) Uiso 1 1 d G . . C253 C 1.0090(4) 0.1126(2) 0.3286(4) 0.021(3) Uiso 1 1 d G . . H25A H 1.0432 0.1357 0.3595 0.026 Uiso 1 1 calc R . . C254 C 1.0385(3) 0.0732(3) 0.3093(4) 0.022(3) Uiso 1 1 d G . . H25B H 1.0929 0.0693 0.3271 0.027 Uiso 1 1 calc R . . C255 C 0.9884(4) 0.0395(2) 0.2640(4) 0.022(3) Uiso 1 1 d G . . H25C H 1.0086 0.0125 0.2509 0.026 Uiso 1 1 calc R . . C256 C 0.9088(3) 0.0451(2) 0.2379(4) 0.017(2) Uiso 1 1 d G . . N261 N 0.7761(4) 0.0197(2) 0.1728(5) 0.036(2) Uani 1 1 d GU . . N262 N 0.7362(3) -0.0201(3) 0.1321(5) 0.037(2) Uani 1 1 d GU . . C263 C 0.7923(5) -0.0527(2) 0.1329(5) 0.035(3) Uiso 1 1 d G . . H26A H 0.7819 -0.0824 0.1099 0.042 Uiso 1 1 calc R . . C264 C 0.8668(4) -0.0332(3) 0.1741(5) 0.028(3) Uiso 1 1 d G . . H26B H 0.9149 -0.0475 0.1836 0.034 Uiso 1 1 calc R . . C265 C 0.8568(4) 0.0116(3) 0.1988(5) 0.025(3) Uiso 1 1 d G . . C271 C 0.6570(9) -0.0248(6) 0.1083(9) 0.041(4) Uiso 1 1 d . . . H27A H 0.6431 -0.0194 0.1507 0.049 Uiso 1 1 calc R . . H27B H 0.6407 -0.0566 0.0889 0.049 Uiso 1 1 calc R . . C272 C 0.6152(7) 0.0117(4) 0.0447(6) 0.052(4) Uiso 1 1 d G . . C273 C 0.5701(7) 0.0464(5) 0.0553(6) 0.067(6) Uiso 1 1 d G . . H27C H 0.5658 0.0486 0.1014 0.080 Uiso 1 1 calc R . . C274 C 0.5315(7) 0.0780(4) -0.0017(8) 0.069(6) Uiso 1 1 d G . . H27D H 0.5007 0.1017 0.0055 0.083 Uiso 1 1 calc R . . C275 C 0.5378(8) 0.0748(5) -0.0693(7) 0.098(8) Uiso 1 1 d G . . C276 C 0.5828(8) 0.0401(5) -0.0798(6) 0.068(6) Uiso 1 1 d G . . H27E H 0.5871 0.0380 -0.1260 0.081 Uiso 1 1 calc R . . C277 C 0.6215(7) 0.0086(4) -0.0228(7) 0.061(5) Uiso 1 1 d G . . H27F H 0.6523 -0.0152 -0.0300 0.073 Uiso 1 1 calc R . . C278 C 0.511(2) 0.1101(12) -0.121(2) 0.140(12) Uiso 1 1 d . . . H27G H 0.4578 0.1179 -0.1268 0.168 Uiso 1 1 calc R . . H27H H 0.5052 0.0973 -0.1697 0.168 Uiso 1 1 calc R . . N281 N 0.6257(8) 0.1605(7) -0.1178(7) 0.113(7) Uani 1 1 d GU . . N282 N 0.5562(7) 0.1561(5) -0.1083(7) 0.113(7) Uani 1 1 d GU . . C283 C 0.5469(10) 0.1970(6) -0.0728(10) 0.110(9) Uiso 1 1 d G . . H28A H 0.5053 0.2033 -0.0597 0.132 Uiso 1 1 calc R . . C284 C 0.6107(12) 0.2266(6) -0.0602(12) 0.128(11) Uiso 1 1 d G . . H28B H 0.6193 0.2563 -0.0373 0.154 Uiso 1 1 calc R . . C285 C 0.6594(8) 0.2041(7) -0.0881(11) 0.115(10) Uiso 1 1 d G . . C292 C 0.7280(11) 0.2071(8) -0.0959(12) 0.143(16) Uani 1 1 d G . . N291 N 0.7438(9) 0.1768(6) -0.1425(10) 0.097(6) Uiso 1 1 d G . . C296 C 0.8150(11) 0.1787(7) -0.1461(10) 0.090(7) Uiso 1 1 d G . . H29A H 0.8258 0.1579 -0.1779 0.108 Uiso 1 1 calc R . . C294 C 0.8703(9) 0.2109(9) -0.1032(15) 0.179(16) Uiso 1 1 d G . . H29B H 0.9190 0.2121 -0.1057 0.215 Uiso 1 1 calc R . . C295 C 0.8545(16) 0.2412(9) -0.0567(15) 0.28(3) Uiso 1 1 d G . . H29C H 0.8923 0.2632 -0.0274 0.338 Uiso 1 1 calc R . . C293 C 0.7833(18) 0.2393(8) -0.0531(14) 0.42(5) Uiso 1 1 d G . . H29D H 0.7725 0.2601 -0.0213 0.503 Uiso 1 1 calc R . . B10 B 0.8460(18) -0.1498(11) 0.4473(18) 0.082(8) Uiso 1 1 d U . . F11 F 0.8423(10) -0.1315(6) 0.3869(10) 0.122(6) Uiso 1 1 d U . . F12 F 0.9110(7) -0.1764(5) 0.4871(7) 0.083(4) Uiso 1 1 d U . . F13 F 0.7836(6) -0.1846(4) 0.4432(6) 0.071(3) Uiso 1 1 d U . . F14 F 0.8413(6) -0.1152(4) 0.4973(6) 0.068(3) Uiso 1 1 d U . . B20 B 0.6563(13) -0.1625(8) 0.0401(12) 0.052(5) Uiso 1 1 d U . . F21 F 0.6614(9) -0.1476(6) 0.1155(9) 0.111(5) Uiso 1 1 d U . . F22 F 0.5847(8) -0.1799(5) 0.0059(8) 0.095(4) Uiso 1 1 d U . . F23 F 0.7128(6) -0.1889(4) 0.0539(6) 0.064(3) Uiso 1 1 d U . . F24 F 0.6622(7) -0.1207(4) 0.0059(7) 0.081(4) Uiso 1 1 d U . . B30 B 1.0204(9) 0.1724(5) 0.8137(9) 0.050 Uiso 1 1 d DU . . F31 F 1.0583(9) 0.1931(6) 0.8840(9) 0.154(7) Uiso 1 1 d DU . . F32 F 1.0284(13) 0.1985(7) 0.7608(11) 0.268(14) Uiso 1 1 d DU . . F33 F 0.9428(8) 0.1643(6) 0.7989(10) 0.161(8) Uiso 1 1 d DU . . F34 F 1.0537(7) 0.1285(4) 0.8178(8) 0.102(5) Uiso 1 1 d DU . . B40 B 1.0779(10) 0.1277(6) 1.0069(10) 0.050 Uiso 0.50 1 d PDU . . F41 F 1.0876(13) 0.1402(8) 1.0779(11) 0.116(10) Uiso 0.50 1 d PDU . . F42 F 1.1480(9) 0.1307(7) 1.0024(10) 0.059(5) Uiso 0.50 1 d PDU . . F43 F 1.0280(10) 0.1605(6) 0.9571(10) 0.065(6) Uiso 0.50 1 d PDU . . F44 F 1.0446(7) 0.0848(4) 0.9901(7) 0.014(3) Uiso 0.50 1 d PDU . . B50 B 0.4241(12) 0.1068(7) -0.4939(11) 0.049(9) Uiso 0.50 1 d PDU . . F51 F 0.3836(14) 0.1172(9) -0.5696(11) 0.124(11) Uiso 0.50 1 d PDU . . F52 F 0.3694(12) 0.1016(8) -0.4647(12) 0.083(7) Uiso 0.50 1 d PDU . . F53 F 0.4717(11) 0.1436(7) -0.4593(11) 0.069(6) Uiso 0.50 1 d PDU . . F54 F 0.4633(14) 0.0653(8) -0.4880(14) 0.086(7) Uiso 0.50 1 d PDU . . C1S C 1.120(2) 0.1645(13) 1.225(2) 0.138(12) Uiso 1 1 d . . . C2S C 0.9703(10) 0.2861(6) 0.2434(10) 0.049(4) Uiso 1 1 d . . . C3S C 0.7497(13) -0.1604(10) 0.2404(13) 0.088(8) Uiso 1 1 d . . . C4S C 1.0452(8) 0.3163(5) 0.2006(8) 0.036(3) Uiso 1 1 d . . . C5S C 0.7859(13) -0.2079(8) 0.2581(12) 0.067(5) Uiso 1 1 d . . . C6S C 0.699(2) -0.1855(13) 0.268(2) 0.141(12) Uiso 1 1 d . . . C7S C 1.0742(17) 0.1346(10) 1.2010(17) 0.102(9) Uiso 1 1 d . . . C8S C 0.9483(17) 0.3467(10) 0.1846(17) 0.106(9) Uiso 1 1 d . . . C9S C 0.6446(11) 0.3139(7) -0.0647(11) 0.061(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0330(6) 0.0300(7) 0.0460(7) -0.0173(5) 0.0141(5) -0.0035(5) Ag2 0.0301(6) 0.0327(7) 0.0460(7) -0.0170(5) 0.0126(5) 0.0093(5) Ag3 0.0670(9) 0.0173(6) 0.0468(7) 0.0213(5) 0.0298(6) 0.0158(5) Ag4 0.1168(17) 0.184(2) 0.0766(13) 0.0744(15) 0.0611(13) 0.1101(17) N111 0.045(7) 0.028(7) 0.030(6) 0.025(5) 0.026(6) 0.026(5) N121 0.048(5) 0.007(4) 0.026(4) 0.006(3) 0.015(4) 0.006(3) N122 0.048(5) 0.007(4) 0.025(4) 0.006(3) 0.015(4) 0.006(3) N141 0.040(5) 0.044(6) 0.041(5) -0.028(4) 0.026(5) -0.013(4) N142 0.041(5) 0.044(6) 0.042(5) -0.028(4) 0.026(5) -0.014(4) N151 0.043(8) 0.081(11) 0.013(6) -0.010(6) 0.008(6) 0.011(7) N161 0.050(6) 0.060(7) 0.032(5) 0.003(5) 0.018(5) 0.041(5) N162 0.050(6) 0.060(7) 0.033(5) 0.003(5) 0.017(5) 0.042(5) N181 0.044(6) 0.080(8) 0.041(6) 0.005(5) 0.021(5) 0.037(5) N182 0.043(6) 0.079(8) 0.041(6) 0.005(5) 0.021(5) 0.038(5) N191 0.079(14) 0.20(3) 0.054(12) 0.032(14) 0.026(11) 0.048(15) N211 0.020(5) 0.018(6) 0.023(5) 0.000(4) 0.014(4) 0.006(4) N221 0.045(6) 0.048(6) 0.030(5) 0.011(4) 0.016(4) 0.009(5) N222 0.046(6) 0.048(6) 0.030(5) 0.010(4) 0.016(4) 0.009(5) N241 0.035(5) 0.020(5) 0.022(4) -0.006(3) 0.004(4) 0.016(3) N242 0.036(5) 0.021(5) 0.022(4) -0.007(3) 0.004(4) 0.016(4) N251 0.005(5) 0.028(7) 0.042(7) -0.004(5) 0.006(5) 0.005(4) N261 0.029(5) 0.016(5) 0.051(6) -0.020(4) 0.006(4) -0.009(4) N262 0.030(5) 0.016(5) 0.052(6) -0.019(4) 0.005(4) -0.009(4) N281 0.071(9) 0.227(18) 0.044(7) 0.071(9) 0.029(7) 0.116(11) N282 0.072(9) 0.227(18) 0.044(7) 0.070(9) 0.029(7) 0.116(11) C292 0.11(2) 0.21(3) 0.17(3) 0.11(3) 0.12(2) 0.13(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N241 2.171(6) . ? Ag1 N141 2.182(8) . ? Ag1 N151 2.493(9) . ? Ag1 C236 2.673(10) . ? Ag1 Ag2 2.8523(17) . ? Ag2 N261 2.184(6) . ? Ag2 N161 2.190(7) . ? Ag2 N251 2.509(5) . ? Ag2 C177 2.659(11) . ? Ag3 N211 2.204(5) . ? Ag3 N111 2.289(6) . ? Ag3 N121 2.323(6) . ? Ag3 N221 2.514(8) . ? Ag4 N191 2.175(16) . ? Ag4 N291 2.196(16) . ? Ag4 N281 2.388(13) . ? Ag4 N181 2.522(8) . ? N111 C112 1.3900 . ? N111 C116 1.3900 . ? C112 C113 1.3900 . ? C112 C125 1.392(8) . ? C113 C114 1.3900 . ? C114 C115 1.3900 . ? C115 C116 1.3900 . ? N121 N122 1.4200 . ? N121 C125 1.4200 . ? N122 C131 1.396(14) . ? N122 C123 1.4200 . ? C123 C124 1.4200 . ? C124 C125 1.4200 . ? C131 C132 1.554(14) . ? C132 C133 1.3900 . ? C132 C137 1.3900 . ? C133 C134 1.3900 . ? C134 C135 1.3900 . ? C135 C136 1.3900 . ? C135 C138 1.463(15) . ? C136 C137 1.3900 . ? C138 N142 1.443(15) . ? N141 N142 1.4200 . ? N141 C145 1.4200 . ? N142 C143 1.4200 . ? C143 C144 1.4200 . ? C144 C145 1.4200 . ? C145 C152 1.343(12) . ? N151 C152 1.3900 . ? N151 C156 1.3900 . ? C152 C153 1.3900 . ? C153 C154 1.3900 . ? C154 C155 1.3900 . ? C155 C156 1.3900 . ? C156 C165 1.376(13) . ? N161 N162 1.4200 . ? N161 C165 1.4200 . ? N162 C163 1.4200 . ? N162 C171 1.470(17) . ? C163 C164 1.4200 . ? C164 C165 1.4200 . ? C171 C172 1.541(17) . ? C172 C173 1.3900 . ? C172 C177 1.3900 . ? C173 C174 1.3900 . ? C174 C175 1.3900 . ? C175 C176 1.3900 . ? C175 C178 1.539(17) . ? C176 C177 1.3900 . ? C178 N182 1.365(18) . ? N181 N182 1.4200 . ? N181 C185 1.4200 . ? N182 C183 1.4200 . ? C183 C184 1.4200 . ? C184 C185 1.4200 . ? C185 C192 1.335(15) . ? N191 C192 1.3900 . ? N191 C196 1.3900 . ? C192 C193 1.3900 . ? C193 C194 1.3900 . ? C194 C195 1.3900 . ? C195 C196 1.3900 . ? N211 C212 1.3900 . ? N211 C216 1.3900 . ? C212 C225 1.370(8) . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C214 C215 1.3900 . ? C215 C216 1.3900 . ? N221 N222 1.4200 . ? N221 C225 1.4200 . ? N222 C231 1.39(2) . ? N222 C223 1.4200 . ? C223 C224 1.4200 . ? C224 C225 1.4200 . ? C231 C232 1.50(2) . ? C232 C233 1.3900 . ? C232 C237 1.3900 . ? C233 C234 1.3900 . ? C234 C235 1.3900 . ? C235 C236 1.3900 . ? C235 C238 1.587(17) . ? C236 C237 1.3900 . ? C238 N242 1.330(16) . ? N241 C245 1.4200 . ? N241 N242 1.4200 . ? N242 C243 1.4200 . ? C243 C244 1.4200 . ? C244 C245 1.4200 . ? C245 C252 1.360(7) . ? N251 C252 1.3900 . ? N251 C256 1.3900 . ? C252 C253 1.3900 . ? C253 C254 1.3900 . ? C254 C255 1.3900 . ? C255 C256 1.3900 . ? C256 C265 1.366(8) . ? N261 N262 1.4200 . ? N261 C265 1.4200 . ? N262 C271 1.385(16) . ? N262 C263 1.4200 . ? C263 C264 1.4200 . ? C264 C265 1.4200 . ? C271 C272 1.570(18) . ? C272 C273 1.3900 . ? C272 C277 1.3900 . ? C273 C274 1.3900 . ? C274 C275 1.3900 . ? C275 C278 1.38(3) . ? C275 C276 1.3900 . ? C276 C277 1.3900 . ? C278 N282 1.55(3) . ? N281 C285 1.4200 . ? N281 N282 1.4200 . ? N282 C283 1.4200 . ? C283 C284 1.4200 . ? C284 C285 1.4200 . ? C285 C292 1.38(2) . ? C292 N291 1.3900 . ? C292 C293 1.3900 . ? N291 C296 1.3900 . ? C296 C294 1.3900 . ? C294 C295 1.3900 . ? C295 C293 1.3900 . ? B10 F11 1.28(3) . ? B10 F12 1.38(3) . ? B10 F14 1.43(3) . ? B10 F13 1.53(3) . ? B20 F23 1.25(2) . ? B20 F22 1.34(2) . ? B20 F24 1.41(2) . ? B20 F21 1.51(3) . ? B30 F32 1.347(16) . ? B30 F31 1.398(16) . ? B30 F34 1.400(15) . ? B30 F33 1.401(16) . ? B40 F44 1.366(15) . ? B40 F42 1.378(15) . ? B40 F41 1.380(15) . ? B40 F43 1.404(15) . ? B50 F53 1.375(15) . ? B50 F54 1.387(15) . ? B50 F51 1.391(15) . ? B50 F52 1.398(15) . ? C1S C7S 1.17(4) . ? C2S C8S 2.04(3) . ? C3S C6S 1.49(4) . ? C3S C5S 1.51(3) . ? C4S C8S 1.94(3) . ? C5S C6S 1.87(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N241 Ag1 N141 166.2(3) . . ? N241 Ag1 N151 120.0(4) . . ? N141 Ag1 N151 71.0(4) . . ? N241 Ag1 C236 76.8(3) . . ? N141 Ag1 C236 110.1(3) . . ? N151 Ag1 C236 102.7(3) . . ? N241 Ag1 Ag2 80.9(2) . . ? N141 Ag1 Ag2 96.8(2) . . ? N151 Ag1 Ag2 69.2(2) . . ? C236 Ag1 Ag2 147.9(2) . . ? N261 Ag2 N161 165.5(4) . . ? N261 Ag2 N251 70.2(3) . . ? N161 Ag2 N251 121.2(3) . . ? N261 Ag2 C177 110.9(3) . . ? N161 Ag2 C177 76.4(3) . . ? N251 Ag2 C177 104.0(2) . . ? N261 Ag2 Ag1 95.6(3) . . ? N161 Ag2 Ag1 81.7(3) . . ? N251 Ag2 Ag1 69.48(18) . . ? C177 Ag2 Ag1 149.1(2) . . ? N211 Ag3 N111 155.3(3) . . ? N211 Ag3 N121 130.5(3) . . ? N111 Ag3 N121 73.9(3) . . ? N211 Ag3 N221 72.4(3) . . ? N111 Ag3 N221 100.7(3) . . ? N121 Ag3 N221 118.2(3) . . ? N191 Ag4 N291 155.4(7) . . ? N191 Ag4 N281 136.7(7) . . ? N291 Ag4 N281 67.2(7) . . ? N191 Ag4 N181 72.4(5) . . ? N291 Ag4 N181 102.9(5) . . ? N281 Ag4 N181 118.8(4) . . ? C112 N111 C116 120.0 . . ? C112 N111 Ag3 115.9(4) . . ? C116 N111 Ag3 122.8(4) . . ? C113 C112 N111 120.0 . . ? C113 C112 C125 123.6(6) . . ? N111 C112 C125 116.2(6) . . ? C112 C113 C114 120.0 . . ? C115 C114 C113 120.0 . . ? C114 C115 C116 120.0 . . ? C115 C116 N111 120.0 . . ? N122 N121 C125 108.0 . . ? N122 N121 Ag3 140.7(4) . . ? C125 N121 Ag3 110.7(4) . . ? C131 N122 N121 118.9(8) . . ? C131 N122 C123 132.6(8) . . ? N121 N122 C123 108.0 . . ? C124 C123 N122 108.0 . . ? C123 C124 C125 108.0 . . ? C112 C125 C124 129.9(6) . . ? C112 C125 N121 122.0(6) . . ? C124 C125 N121 108.0 . . ? N122 C131 C132 112.2(9) . . ? C133 C132 C137 120.0 . . ? C133 C132 C131 121.1(7) . . ? C137 C132 C131 118.9(7) . . ? C132 C133 C134 120.0 . . ? C135 C134 C133 120.0 . . ? C134 C135 C136 120.0 . . ? C134 C135 C138 119.2(8) . . ? C136 C135 C138 120.8(8) . . ? C137 C136 C135 120.0 . . ? C136 C137 C132 120.0 . . ? N142 C138 C135 113.7(11) . . ? N142 N141 C145 108.0 . . ? N142 N141 Ag1 133.1(6) . . ? C145 N141 Ag1 117.5(6) . . ? N141 N142 C143 108.0 . . ? N141 N142 C138 120.5(9) . . ? C143 N142 C138 131.5(9) . . ? C144 C143 N142 108.0 . . ? C143 C144 C145 108.0 . . ? C152 C145 C144 132.2(10) . . ? C152 C145 N141 119.5(10) . . ? C144 C145 N141 108.0 . . ? C152 N151 C156 120.0 . . ? C152 N151 Ag1 108.4(7) . . ? C156 N151 Ag1 129.6(7) . . ? C145 C152 C153 120.5(10) . . ? C145 C152 N151 119.5(10) . . ? C153 C152 N151 120.0 . . ? C154 C153 C152 120.0 . . ? C153 C154 C155 120.0 . . ? C156 C155 C154 120.0 . . ? C165 C156 C155 119.6(10) . . ? C165 C156 N151 119.6(10) . . ? C155 C156 N151 120.0 . . ? N162 N161 C165 108.0 . . ? N162 N161 Ag2 123.1(6) . . ? C165 N161 Ag2 126.9(6) . . ? N161 N162 C163 108.0 . . ? N161 N162 C171 123.8(10) . . ? C163 N162 C171 128.1(10) . . ? C164 C163 N162 108.0 . . ? C163 C164 C165 108.0 . . ? C156 C165 C164 131.1(10) . . ? C156 C165 N161 120.7(10) . . ? C164 C165 N161 108.0 . . ? N162 C171 C172 108.4(12) . . ? C173 C172 C177 120.0 . . ? C173 C172 C171 112.9(8) . . ? C177 C172 C171 126.8(8) . . ? C172 C173 C174 120.0 . . ? C173 C174 C175 120.0 . . ? C176 C175 C174 120.0 . . ? C176 C175 C178 122.9(8) . . ? C174 C175 C178 117.0(8) . . ? C175 C176 C177 120.0 . . ? C176 C177 C172 120.0 . . ? C176 C177 Ag2 102.7(4) . . ? C172 C177 Ag2 85.7(4) . . ? N182 C178 C175 113.4(12) . . ? N182 N181 C185 108.0 . . ? N182 N181 Ag4 138.6(6) . . ? C185 N181 Ag4 102.9(6) . . ? C178 N182 N181 120.0(10) . . ? C178 N182 C183 131.9(10) . . ? N181 N182 C183 108.0 . . ? C184 C183 N182 108.0 . . ? C185 C184 C183 108.0 . . ? C192 C185 C184 131.8(12) . . ? C192 C185 N181 120.2(12) . . ? C184 C185 N181 108.0 . . ? C192 N191 C196 120.0 . . ? C192 N191 Ag4 117.3(11) . . ? C196 N191 Ag4 122.7(11) . . ? C185 C192 N191 120.2(15) . . ? C185 C192 C193 119.8(15) . . ? N191 C192 C193 120.0 . . ? C194 C193 C192 120.0 . . ? C193 C194 C195 120.0 . . ? C196 C195 C194 120.0 . . ? C195 C196 N191 120.0 . . ? C212 N211 C216 120.0 . . ? C212 N211 Ag3 118.2(3) . . ? C216 N211 Ag3 121.8(3) . . ? C225 C212 C213 121.0(6) . . ? C225 C212 N211 119.0(6) . . ? C213 C212 N211 120.0 . . ? C212 C213 C214 120.0 . . ? C215 C214 C213 120.0 . . ? C214 C215 C216 120.0 . . ? C215 C216 N211 120.0 . . ? N222 N221 C225 108.0 . . ? N222 N221 Ag3 139.2(5) . . ? C225 N221 Ag3 104.6(5) . . ? C231 N222 N221 120.2(11) . . ? C231 N222 C223 131.5(11) . . ? N221 N222 C223 108.0 . . ? C224 C223 N222 108.0 . . ? C223 C224 C225 108.0 . . ? C212 C225 N221 120.2(7) . . ? C212 C225 C224 131.8(7) . . ? N221 C225 C224 108.0 . . ? N222 C231 C232 115.8(15) . . ? C233 C232 C237 120.0 . . ? C233 C232 C231 118.2(10) . . ? C237 C232 C231 121.7(10) . . ? C232 C233 C234 120.0 . . ? C235 C234 C233 120.0 . . ? C234 C235 C236 120.0 . . ? C234 C235 C238 120.8(8) . . ? C236 C235 C238 119.2(8) . . ? C235 C236 C237 120.0 . . ? C235 C236 Ag1 87.8(4) . . ? C237 C236 Ag1 102.4(4) . . ? C236 C237 C232 120.0 . . ? N242 C238 C235 114.9(12) . . ? C245 N241 N242 108.0 . . ? C245 N241 Ag1 127.0(4) . . ? N242 N241 Ag1 122.8(4) . . ? C238 N242 N241 123.4(9) . . ? C238 N242 C243 128.0(9) . . ? N241 N242 C243 108.0 . . ? C244 C243 N242 108.0 . . ? C243 C244 C245 108.0 . . ? C252 C245 C244 130.5(6) . . ? C252 C245 N241 121.3(6) . . ? C244 C245 N241 108.0 . . ? C252 N251 C256 120.0 . . ? C252 N251 Ag2 128.8(3) . . ? C256 N251 Ag2 109.2(3) . . ? C245 C252 N251 118.4(6) . . ? C245 C252 C253 121.6(6) . . ? N251 C252 C253 120.0 . . ? C254 C253 C252 120.0 . . ? C255 C254 C253 120.0 . . ? C254 C255 C256 120.0 . . ? C265 C256 C255 122.9(6) . . ? C265 C256 N251 116.8(6) . . ? C255 C256 N251 120.0 . . ? N262 N261 C265 108.0 . . ? N262 N261 Ag2 131.4(4) . . ? C265 N261 Ag2 118.0(4) . . ? C271 N262 C263 130.3(9) . . ? C271 N262 N261 121.0(9) . . ? C263 N262 N261 108.0 . . ? N262 C263 C264 108.0 . . ? C265 C264 C263 108.0 . . ? C256 C265 C264 131.7(6) . . ? C256 C265 N261 120.3(6) . . ? C264 C265 N261 108.0 . . ? N262 C271 C272 108.5(12) . . ? C273 C272 C277 120.0 . . ? C273 C272 C271 120.0(10) . . ? C277 C272 C271 120.0(10) . . ? C274 C273 C272 120.0 . . ? C273 C274 C275 120.0 . . ? C278 C275 C276 118.8(19) . . ? C278 C275 C274 120.3(19) . . ? C276 C275 C274 120.0 . . ? C275 C276 C277 120.0 . . ? C276 C277 C272 120.0 . . ? C275 C278 N282 120(3) . . ? C285 N281 N282 108.0 . . ? C285 N281 Ag4 121.2(11) . . ? N282 N281 Ag4 130.1(11) . . ? N281 N282 C283 108.0 . . ? N281 N282 C278 123.2(17) . . ? C283 N282 C278 127.8(18) . . ? N282 C283 C284 108.0 . . ? C285 C284 C283 108.0 . . ? C292 C285 C284 144.9(19) . . ? C292 C285 N281 107.0(19) . . ? C284 C285 N281 108.0 . . ? C285 C292 N291 121(2) . . ? C285 C292 C293 119(2) . . ? N291 C292 C293 120.0 . . ? C292 N291 C296 120.0 . . ? C292 N291 Ag4 121.9(13) . . ? C296 N291 Ag4 115.9(13) . . ? N291 C296 C294 120.0 . . ? C295 C294 C296 120.0 . . ? C294 C295 C293 120.0 . . ? C295 C293 C292 120.0 . . ? F11 B10 F12 116(3) . . ? F11 B10 F14 111(2) . . ? F12 B10 F14 107(2) . . ? F11 B10 F13 119(2) . . ? F12 B10 F13 99(2) . . ? F14 B10 F13 103(2) . . ? F23 B20 F22 118.9(19) . . ? F23 B20 F24 112.9(18) . . ? F22 B20 F24 110.6(18) . . ? F23 B20 F21 105.6(17) . . ? F22 B20 F21 103.1(17) . . ? F24 B20 F21 104.1(16) . . ? F32 B30 F31 110.4(12) . . ? F32 B30 F34 110.7(13) . . ? F31 B30 F34 107.3(11) . . ? F32 B30 F33 112.8(13) . . ? F31 B30 F33 109.5(12) . . ? F34 B30 F33 106.0(11) . . ? F44 B40 F42 113.9(16) . . ? F44 B40 F41 109.3(12) . . ? F42 B40 F41 109.4(12) . . ? F44 B40 F43 109.4(11) . . ? F42 B40 F43 107.5(11) . . ? F41 B40 F43 107.1(12) . . ? F53 B50 F54 114(2) . . ? F53 B50 F51 108.4(13) . . ? F54 B50 F51 108.1(13) . . ? F53 B50 F52 109.1(12) . . ? F54 B50 F52 110(2) . . ? F51 B50 F52 107.0(13) . . ? C6S C3S C5S 77(2) . . ? C3S C5S C6S 51.0(14) . . ? C3S C6S C5S 51.9(15) . . ? C4S C8S C2S 64.5(11) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.000 _refine_diff_density_min -5.178 _refine_diff_density_rms 0.254