#Electronic Supplementary Material for Dalton Transactions #This Journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Suning Wang' _publ_contact_author_email WANGS@CHEM.QUEENSU.CA _publ_section_title ; Cu(I) and Ag(I) Complexes of 7-Azaindolyl and 2,2'-dipyridylamino Substituted 1,3,5-Triazine and Benzene: The central core impact on Structure, Solution Dynamics and Fluorescence of the Complexes ; loop_ _publ_author_name 'Suning Wang.' 'John Li' 'Corey Seward' 'Elizabeth Wong' # Attachment '1.cif' data_jli5 _database_code_depnum_ccdc_archive 'CCDC 699116' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H30 B Cu F4 N9 P' _chemical_formula_weight 842.07 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' 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 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 15.009(4) _cell_length_b 14.840(4) _cell_length_c 17.565(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.363(6) _cell_angle_gamma 90.00 _cell_volume 3870.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8244 _exptl_absorpt_correction_T_max 0.8777 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _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 20499 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7602 _reflns_number_gt 5236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0390P)^2^+3.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7602 _refine_ls_number_parameters 532 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.070 _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 P1 P 0.21116(5) 0.46976(5) -0.07950(4) 0.03767(19) Uani 1 1 d . . . Cu1 Cu 0.16992(2) 0.35053(3) -0.15154(2) 0.04121(12) Uani 1 1 d . . . N1 N -0.04228(16) 0.35030(17) -0.22119(14) 0.0435(6) Uani 1 1 d . . . N2 N 0.07169(17) 0.26216(16) -0.13936(13) 0.0415(6) Uani 1 1 d . . . N3 N 0.22487(17) 0.41952(17) -0.31482(13) 0.0437(6) Uani 1 1 d . . . N4 N 0.27494(17) 0.31629(17) -0.20848(13) 0.0445(6) Uani 1 1 d . . . N5 N -0.03787(17) 0.56884(18) -0.40650(14) 0.0481(7) Uani 1 1 d . . . N6 N 0.07683(19) 0.61928(18) -0.48167(15) 0.0511(7) Uani 1 1 d . . . N7 N 0.09562(16) 0.38930(17) -0.25930(13) 0.0412(6) Uani 1 1 d . . . N8 N 0.09455(17) 0.49437(18) -0.36185(14) 0.0471(6) Uani 1 1 d . . . N9 N -0.04097(17) 0.46121(18) -0.31246(14) 0.0470(6) Uani 1 1 d . . . C1 C -0.1282(2) 0.5907(3) -0.4068(2) 0.0620(10) Uani 1 1 d . . . H1A H -0.1657 0.5639 -0.3756 0.074 Uiso 1 1 calc R . . C2 C -0.1535(3) 0.6557(3) -0.4584(2) 0.0714(11) Uani 1 1 d . . . H2A H -0.2102 0.6819 -0.4684 0.086 Uiso 1 1 calc R . . C3 C -0.0768(2) 0.6775(2) -0.49553(19) 0.0551(9) Uani 1 1 d . . . C4 C -0.0598(3) 0.7362(3) -0.5525(2) 0.0706(11) Uani 1 1 d . . . H4A H -0.1040 0.7750 -0.5760 0.085 Uiso 1 1 calc R . . C5 C 0.0252(3) 0.7351(3) -0.5735(2) 0.0688(11) Uani 1 1 d . . . H5A H 0.0393 0.7737 -0.6118 0.083 Uiso 1 1 calc R . . C6 C 0.0891(3) 0.6769(2) -0.5376(2) 0.0610(9) Uani 1 1 d . . . H6B H 0.1455 0.6777 -0.5535 0.073 Uiso 1 1 calc R . . C7 C -0.0059(2) 0.6219(2) -0.46301(17) 0.0466(8) Uani 1 1 d . . . C8 C 0.2691(2) 0.4592(2) -0.37222(18) 0.0521(8) Uani 1 1 d . . . H8B H 0.2426 0.4989 -0.4099 0.062 Uiso 1 1 calc R . . C9 C 0.3540(2) 0.4313(2) -0.36438(19) 0.0552(9) Uani 1 1 d . . . H9B H 0.3965 0.4480 -0.3954 0.066 Uiso 1 1 calc R . . C10 C 0.3693(2) 0.3709(2) -0.29976(18) 0.0502(8) Uani 1 1 d . . . C11 C 0.4424(2) 0.3229(3) -0.2640(2) 0.0626(10) Uani 1 1 d . . . H11A H 0.4980 0.3257 -0.2814 0.075 Uiso 1 1 calc R . . C12 C 0.4297(2) 0.2706(3) -0.2015(2) 0.0672(11) Uani 1 1 d . . . H12A H 0.4769 0.2361 -0.1767 0.081 Uiso 1 1 calc R . . C13 C 0.3475(2) 0.2693(2) -0.1760(2) 0.0593(9) Uani 1 1 d . . . H13A H 0.3414 0.2336 -0.1335 0.071 Uiso 1 1 calc R . . C14 C 0.2883(2) 0.3644(2) -0.26976(17) 0.0434(7) Uani 1 1 d . . . C15 C -0.1374(2) 0.3477(2) -0.23419(19) 0.0517(8) Uani 1 1 d . . . H15A H -0.1740 0.3875 -0.2654 0.062 Uiso 1 1 calc R . . C16 C -0.1666(2) 0.2798(2) -0.19509(19) 0.0555(9) Uani 1 1 d . . . H16A H -0.2266 0.2646 -0.1943 0.067 Uiso 1 1 calc R . . C17 C -0.0901(2) 0.2340(2) -0.15446(17) 0.0459(8) Uani 1 1 d . . . C18 C -0.0774(3) 0.1599(2) -0.10660(19) 0.0559(9) Uani 1 1 d . . . H18A H -0.1259 0.1257 -0.0957 0.067 Uiso 1 1 calc R . . C19 C 0.0094(3) 0.1385(2) -0.07558(19) 0.0563(9) Uani 1 1 d . . . H19A H 0.0202 0.0888 -0.0434 0.068 Uiso 1 1 calc R . . C20 C 0.0806(2) 0.1904(2) -0.09184(17) 0.0494(8) Uani 1 1 d . . . H20A H 0.1382 0.1749 -0.0686 0.059 Uiso 1 1 calc R . . C21 C -0.0132(2) 0.2799(2) -0.17041(16) 0.0413(7) Uani 1 1 d . . . C22 C 0.0064(2) 0.4025(2) -0.26558(16) 0.0411(7) Uani 1 1 d . . . C23 C 0.0080(2) 0.5050(2) -0.35792(17) 0.0432(7) Uani 1 1 d . . . C24 C 0.1345(2) 0.4346(2) -0.31105(16) 0.0424(7) Uani 1 1 d . . . C25 C 0.1240(2) 0.5554(2) -0.08035(16) 0.0428(7) Uani 1 1 d . . . C26 C 0.1403(3) 0.6467(2) -0.06718(19) 0.0562(9) Uani 1 1 d . . . H26A H 0.1992 0.6681 -0.0588 0.067 Uiso 1 1 calc R . . C27 C 0.0692(3) 0.7059(3) -0.0665(2) 0.0700(11) Uani 1 1 d . . . H27A H 0.0804 0.7667 -0.0566 0.084 Uiso 1 1 calc R . . C28 C -0.0181(3) 0.6752(3) -0.0804(2) 0.0764(12) Uani 1 1 d . . . H28A H -0.0656 0.7153 -0.0804 0.092 Uiso 1 1 calc R . . C29 C -0.0351(3) 0.5864(3) -0.0941(2) 0.0707(11) Uani 1 1 d . . . H29A H -0.0942 0.5660 -0.1039 0.085 Uiso 1 1 calc R . . C30 C 0.0352(2) 0.5259(2) -0.09345(18) 0.0527(8) Uani 1 1 d . . . H30A H 0.0229 0.4650 -0.1019 0.063 Uiso 1 1 calc R . . C31 C 0.3026(2) 0.5256(2) -0.11881(16) 0.0418(7) Uani 1 1 d . . . C32 C 0.3912(2) 0.4999(3) -0.0944(2) 0.0570(9) Uani 1 1 d . . . H32A H 0.4048 0.4628 -0.0516 0.068 Uiso 1 1 calc R . . C33 C 0.4591(3) 0.5293(3) -0.1337(2) 0.0703(11) Uani 1 1 d . . . H33A H 0.5182 0.5117 -0.1172 0.084 Uiso 1 1 calc R . . C34 C 0.4400(3) 0.5844(3) -0.1969(2) 0.0690(11) Uani 1 1 d . . . H34A H 0.4859 0.6031 -0.2235 0.083 Uiso 1 1 calc R . . C35 C 0.3537(3) 0.6114(3) -0.2203(2) 0.0651(10) Uani 1 1 d . . . H35A H 0.3410 0.6499 -0.2623 0.078 Uiso 1 1 calc R . . C36 C 0.2850(2) 0.5823(2) -0.18237(18) 0.0515(8) Uani 1 1 d . . . H36A H 0.2262 0.6006 -0.1994 0.062 Uiso 1 1 calc R . . C37 C 0.25318(19) 0.4538(2) 0.02244(16) 0.0401(7) Uani 1 1 d . . . C38 C 0.2533(2) 0.3676(2) 0.05193(18) 0.0490(8) Uani 1 1 d . . . H38A H 0.2369 0.3193 0.0191 0.059 Uiso 1 1 calc R . . C39 C 0.2778(2) 0.3522(3) 0.13021(19) 0.0608(9) Uani 1 1 d . . . H39A H 0.2778 0.2940 0.1497 0.073 Uiso 1 1 calc R . . C40 C 0.3018(2) 0.4231(3) 0.17829(19) 0.0608(10) Uani 1 1 d . . . H40A H 0.3176 0.4128 0.2307 0.073 Uiso 1 1 calc R . . C41 C 0.3030(2) 0.5093(3) 0.15032(19) 0.0614(10) Uani 1 1 d . . . H41A H 0.3201 0.5571 0.1835 0.074 Uiso 1 1 calc R . . C42 C 0.2786(2) 0.5246(2) 0.07221(18) 0.0539(9) Uani 1 1 d . . . H42A H 0.2793 0.5829 0.0531 0.065 Uiso 1 1 calc R . . B1 B 0.3416(3) 0.5839(4) -0.6140(3) 0.0860(18) Uani 1 1 d D . . F1 F 0.29013(16) 0.52422(17) -0.65715(14) 0.0876(7) Uani 1 1 d D . . F2 F 0.42918(17) 0.5752(2) -0.60644(17) 0.1142(10) Uani 1 1 d D . . F3 F 0.3053(2) 0.6477(2) -0.5797(2) 0.1317(12) Uani 1 1 d D . . F5 F 0.3442(3) 0.6514(3) -0.6859(3) 0.0926(15) Uani 0.50 1 d PD . . F5A F 0.3407(4) 0.5268(4) -0.5380(3) 0.1064(18) Uani 0.50 1 d PD . . 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 P1 0.0372(4) 0.0396(4) 0.0359(4) -0.0003(3) 0.0042(3) -0.0001(4) Cu1 0.0436(2) 0.0413(2) 0.03728(19) 0.00175(17) 0.00102(15) 0.00080(18) N1 0.0430(14) 0.0438(15) 0.0427(13) 0.0058(12) 0.0026(11) -0.0024(13) N2 0.0488(16) 0.0379(14) 0.0370(13) 0.0000(11) 0.0030(11) 0.0005(12) N3 0.0450(15) 0.0476(16) 0.0386(13) 0.0059(12) 0.0068(11) 0.0031(13) N4 0.0511(16) 0.0437(15) 0.0387(14) 0.0026(12) 0.0071(12) 0.0099(13) N5 0.0448(16) 0.0464(16) 0.0510(15) 0.0120(13) 0.0001(12) 0.0035(13) N6 0.0538(17) 0.0497(17) 0.0487(15) 0.0077(13) 0.0034(13) 0.0023(14) N7 0.0419(15) 0.0431(15) 0.0369(13) 0.0044(11) -0.0003(11) 0.0004(12) N8 0.0454(16) 0.0485(16) 0.0466(15) 0.0124(13) 0.0043(12) 0.0029(13) N9 0.0449(15) 0.0455(16) 0.0489(15) 0.0076(13) 0.0012(12) 0.0005(13) C1 0.046(2) 0.066(2) 0.073(2) 0.024(2) 0.0060(17) 0.0050(19) C2 0.052(2) 0.078(3) 0.083(3) 0.028(2) 0.0055(19) 0.017(2) C3 0.059(2) 0.049(2) 0.0542(19) 0.0121(16) -0.0026(16) 0.0073(17) C4 0.076(3) 0.063(3) 0.071(2) 0.027(2) 0.004(2) 0.016(2) C5 0.079(3) 0.063(3) 0.065(2) 0.022(2) 0.012(2) 0.004(2) C6 0.068(2) 0.061(2) 0.054(2) 0.0085(18) 0.0096(18) -0.003(2) C7 0.054(2) 0.0417(18) 0.0409(17) 0.0026(14) -0.0026(15) -0.0013(16) C8 0.055(2) 0.057(2) 0.0451(18) 0.0101(16) 0.0106(15) 0.0037(18) C9 0.054(2) 0.063(2) 0.0513(19) 0.0065(17) 0.0183(16) -0.0022(18) C10 0.0490(19) 0.054(2) 0.0482(18) -0.0035(15) 0.0081(15) 0.0048(17) C11 0.051(2) 0.080(3) 0.060(2) 0.000(2) 0.0173(17) 0.011(2) C12 0.055(2) 0.076(3) 0.071(2) 0.014(2) 0.0107(19) 0.026(2) C13 0.063(2) 0.061(2) 0.054(2) 0.0127(18) 0.0117(17) 0.018(2) C14 0.0460(18) 0.0441(19) 0.0397(16) -0.0032(14) 0.0050(13) 0.0057(15) C15 0.0398(18) 0.061(2) 0.0531(19) 0.0044(17) 0.0024(14) 0.0008(17) C16 0.046(2) 0.064(2) 0.057(2) -0.0002(18) 0.0086(16) -0.0101(18) C17 0.0503(19) 0.0460(19) 0.0421(16) -0.0066(15) 0.0091(14) -0.0091(16) C18 0.066(2) 0.047(2) 0.056(2) 0.0004(17) 0.0151(17) -0.0130(18) C19 0.076(3) 0.0411(19) 0.0526(19) 0.0070(16) 0.0118(18) -0.0033(19) C20 0.058(2) 0.0439(19) 0.0450(18) 0.0036(15) 0.0041(15) 0.0015(17) C21 0.0518(19) 0.0366(17) 0.0348(15) -0.0040(13) 0.0043(13) -0.0018(15) C22 0.0433(18) 0.0426(18) 0.0353(15) -0.0023(14) -0.0018(13) 0.0003(15) C23 0.0465(19) 0.0391(18) 0.0419(16) -0.0003(14) -0.0004(14) 0.0007(15) C24 0.0470(19) 0.0405(18) 0.0383(16) -0.0011(14) 0.0013(14) 0.0005(15) C25 0.0475(19) 0.0449(19) 0.0367(15) 0.0023(13) 0.0083(13) 0.0061(15) C26 0.063(2) 0.047(2) 0.060(2) 0.0011(17) 0.0117(17) 0.0021(19) C27 0.100(3) 0.045(2) 0.070(2) 0.0038(18) 0.027(2) 0.017(2) C28 0.078(3) 0.076(3) 0.080(3) 0.012(2) 0.027(2) 0.035(3) C29 0.051(2) 0.080(3) 0.083(3) 0.000(2) 0.0150(19) 0.017(2) C30 0.046(2) 0.054(2) 0.058(2) -0.0021(17) 0.0098(16) 0.0055(17) C31 0.0437(18) 0.0426(18) 0.0396(16) -0.0070(14) 0.0081(13) -0.0054(15) C32 0.048(2) 0.069(2) 0.0538(19) 0.0001(18) 0.0080(16) -0.0007(18) C33 0.047(2) 0.086(3) 0.079(3) -0.008(2) 0.0152(19) -0.006(2) C34 0.068(3) 0.075(3) 0.071(3) -0.012(2) 0.036(2) -0.023(2) C35 0.083(3) 0.065(2) 0.052(2) 0.0022(18) 0.024(2) -0.014(2) C36 0.055(2) 0.054(2) 0.0454(18) 0.0008(16) 0.0090(15) -0.0034(17) C37 0.0367(16) 0.0470(19) 0.0367(15) -0.0018(14) 0.0057(12) 0.0040(14) C38 0.053(2) 0.051(2) 0.0426(17) 0.0002(15) 0.0054(14) 0.0062(16) C39 0.070(2) 0.063(2) 0.0485(19) 0.0098(19) 0.0067(17) 0.010(2) C40 0.060(2) 0.083(3) 0.0386(18) 0.0068(19) 0.0046(16) 0.015(2) C41 0.063(2) 0.075(3) 0.0440(19) -0.0149(18) -0.0009(16) 0.005(2) C42 0.061(2) 0.050(2) 0.0482(19) -0.0011(16) 0.0004(16) 0.0003(18) B1 0.045(3) 0.083(4) 0.122(5) -0.052(4) -0.015(3) 0.017(3) F1 0.0845(16) 0.0882(18) 0.0849(16) -0.0157(14) -0.0048(13) -0.0079(14) F2 0.0619(16) 0.141(3) 0.139(2) -0.022(2) 0.0112(15) 0.0064(17) F3 0.103(2) 0.124(3) 0.167(3) -0.066(2) 0.016(2) 0.0222(19) F5 0.078(3) 0.078(3) 0.116(4) 0.013(3) -0.004(3) -0.010(3) F5A 0.149(5) 0.109(4) 0.056(3) 0.011(3) -0.003(3) -0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C25 1.822(3) . ? P1 C31 1.823(3) . ? P1 C37 1.825(3) . ? P1 Cu1 2.2106(10) . ? Cu1 N2 2.008(3) . ? Cu1 N4 2.050(2) . ? Cu1 N7 2.132(2) . ? N1 C22 1.382(4) . ? N1 C21 1.401(4) . ? N1 C15 1.413(4) . ? N2 C21 1.338(4) . ? N2 C20 1.348(4) . ? N3 C24 1.385(4) . ? N3 C14 1.408(4) . ? N3 C8 1.414(4) . ? N4 C14 1.331(4) . ? N4 C13 1.348(4) . ? N5 C23 1.388(4) . ? N5 C1 1.393(4) . ? N5 C7 1.405(4) . ? N6 C7 1.331(4) . ? N6 C6 1.335(4) . ? N7 C24 1.332(4) . ? N7 C22 1.341(4) . ? N8 C23 1.321(4) . ? N8 C24 1.337(4) . ? N9 C23 1.331(4) . ? N9 C22 1.331(4) . ? C1 C2 1.340(5) . ? C2 C3 1.439(5) . ? C3 C4 1.378(5) . ? C3 C7 1.401(4) . ? C4 C5 1.379(5) . ? C5 C6 1.374(5) . ? C8 C9 1.329(4) . ? C9 C10 1.438(5) . ? C10 C11 1.380(5) . ? C10 C14 1.397(4) . ? C11 C12 1.381(5) . ? C12 C13 1.373(5) . ? C15 C16 1.330(5) . ? C16 C17 1.433(5) . ? C17 C18 1.380(4) . ? C17 C21 1.403(4) . ? C18 C19 1.374(5) . ? C19 C20 1.380(5) . ? C25 C30 1.390(4) . ? C25 C26 1.391(4) . ? C26 C27 1.385(5) . ? C27 C28 1.375(6) . ? C28 C29 1.357(6) . ? C29 C30 1.383(5) . ? C31 C32 1.390(4) . ? C31 C36 1.392(4) . ? C32 C33 1.382(5) . ? C33 C34 1.374(5) . ? C34 C35 1.362(5) . ? C35 C36 1.377(5) . ? C37 C38 1.381(4) . ? C37 C42 1.384(4) . ? C38 C39 1.389(4) . ? C39 C40 1.364(5) . ? C40 C41 1.371(5) . ? C41 C42 1.386(4) . ? B1 F3 1.284(5) . ? B1 F2 1.308(5) . ? B1 F1 1.337(5) . ? B1 F5A 1.583(8) . ? B1 F5 1.617(8) . ? 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 C25 P1 C31 105.01(15) . . ? C25 P1 C37 104.09(13) . . ? C31 P1 C37 104.99(14) . . ? C25 P1 Cu1 114.36(11) . . ? C31 P1 Cu1 108.10(10) . . ? C37 P1 Cu1 119.07(11) . . ? N2 Cu1 N4 121.25(10) . . ? N2 Cu1 N7 88.48(10) . . ? N4 Cu1 N7 88.49(10) . . ? N2 Cu1 P1 127.64(7) . . ? N4 Cu1 P1 107.85(8) . . ? N7 Cu1 P1 111.04(7) . . ? C22 N1 C21 129.5(3) . . ? C22 N1 C15 121.9(3) . . ? C21 N1 C15 107.2(3) . . ? C21 N2 C20 114.3(3) . . ? C21 N2 Cu1 119.9(2) . . ? C20 N2 Cu1 125.0(2) . . ? C24 N3 C14 130.8(2) . . ? C24 N3 C8 122.1(3) . . ? C14 N3 C8 107.1(2) . . ? C14 N4 C13 114.4(3) . . ? C14 N4 Cu1 118.6(2) . . ? C13 N4 Cu1 123.5(2) . . ? C23 N5 C1 123.8(3) . . ? C23 N5 C7 128.8(3) . . ? C1 N5 C7 107.4(3) . . ? C7 N6 C6 113.3(3) . . ? C24 N7 C22 113.7(3) . . ? C24 N7 Cu1 121.2(2) . . ? C22 N7 Cu1 119.96(19) . . ? C23 N8 C24 113.2(3) . . ? C23 N9 C22 113.5(3) . . ? C2 C1 N5 110.5(3) . . ? C1 C2 C3 107.6(3) . . ? C4 C3 C7 117.2(3) . . ? C4 C3 C2 135.8(3) . . ? C7 C3 C2 107.0(3) . . ? C3 C4 C5 117.7(3) . . ? C6 C5 C4 119.7(3) . . ? N6 C6 C5 125.4(4) . . ? N6 C7 C3 126.7(3) . . ? N6 C7 N5 125.8(3) . . ? C3 C7 N5 107.5(3) . . ? C9 C8 N3 109.8(3) . . ? C8 C9 C10 108.4(3) . . ? C11 C10 C14 118.1(3) . . ? C11 C10 C9 134.9(3) . . ? C14 C10 C9 107.0(3) . . ? C10 C11 C12 117.3(3) . . ? C13 C12 C11 120.2(3) . . ? N4 C13 C12 124.3(3) . . ? N4 C14 C10 125.7(3) . . ? N4 C14 N3 126.6(3) . . ? C10 C14 N3 107.6(3) . . ? C16 C15 N1 109.8(3) . . ? C15 C16 C17 108.4(3) . . ? C18 C17 C21 117.6(3) . . ? C18 C17 C16 135.3(3) . . ? C21 C17 C16 107.1(3) . . ? C19 C18 C17 117.7(3) . . ? C18 C19 C20 120.5(3) . . ? N2 C20 C19 124.0(3) . . ? N2 C21 N1 126.6(3) . . ? N2 C21 C17 125.8(3) . . ? N1 C21 C17 107.5(3) . . ? N9 C22 N7 125.7(3) . . ? N9 C22 N1 115.9(3) . . ? N7 C22 N1 118.4(3) . . ? N8 C23 N9 127.3(3) . . ? N8 C23 N5 116.9(3) . . ? N9 C23 N5 115.8(3) . . ? N7 C24 N8 126.3(3) . . ? N7 C24 N3 118.7(3) . . ? N8 C24 N3 115.0(3) . . ? C30 C25 C26 118.4(3) . . ? C30 C25 P1 116.9(2) . . ? C26 C25 P1 124.7(3) . . ? C27 C26 C25 120.1(4) . . ? C28 C27 C26 120.3(4) . . ? C29 C28 C27 120.2(4) . . ? C28 C29 C30 120.3(4) . . ? C29 C30 C25 120.6(3) . . ? C32 C31 C36 118.4(3) . . ? C32 C31 P1 119.8(3) . . ? C36 C31 P1 120.8(2) . . ? C33 C32 C31 120.1(3) . . ? C34 C33 C32 120.6(4) . . ? C35 C34 C33 119.8(3) . . ? C34 C35 C36 120.5(4) . . ? C35 C36 C31 120.7(3) . . ? C38 C37 C42 118.7(3) . . ? C38 C37 P1 118.0(2) . . ? C42 C37 P1 123.1(2) . . ? C37 C38 C39 120.6(3) . . ? C40 C39 C38 119.6(3) . . ? C39 C40 C41 120.9(3) . . ? C40 C41 C42 119.5(3) . . ? C37 C42 C41 120.7(3) . . ? F3 B1 F2 120.9(4) . . ? F3 B1 F1 120.3(4) . . ? F2 B1 F1 118.8(4) . . ? F3 B1 F5A 86.7(5) . . ? F2 B1 F5A 89.6(4) . . ? F1 B1 F5A 92.8(4) . . ? F3 B1 F5 88.3(4) . . ? F2 B1 F5 90.1(4) . . ? F1 B1 F5 92.6(4) . . ? F5A B1 F5 174.0(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.525 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.053 # Attachment '2.cif' data_jli4b _database_code_depnum_ccdc_archive 'CCDC 699117' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H35 B Cl2 Cu F4 N6 P' _chemical_formula_weight 924.02 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' 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' Cl Cl 0.1484 0.1585 '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 12.115(4) _cell_length_b 14.578(4) _cell_length_c 23.231(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.189(5) _cell_angle_gamma 90.00 _cell_volume 4100(2) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rectangle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8033 _exptl_absorpt_correction_T_max 0.8623 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 P4' _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 19058 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8002 _reflns_number_gt 5160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0580P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8002 _refine_ls_number_parameters 553 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 B1 B 0.4988(4) 0.1962(3) 0.1406(2) 0.0476(12) Uani 1 1 d . . . P1 P 0.89846(7) 0.26010(5) 0.31926(4) 0.0254(2) Uani 1 1 d . . . Cu1 Cu 0.89426(3) 0.15718(3) 0.248329(16) 0.02613(12) Uani 1 1 d . . . N1 N 1.3147(2) 0.15085(19) 0.32257(12) 0.0356(7) Uani 1 1 d . . . N2 N 1.2492(3) 0.1632(2) 0.41868(14) 0.0520(9) Uani 1 1 d . . . N3 N 0.9742(2) -0.02762(16) 0.32225(11) 0.0281(6) Uani 1 1 d . . . N4 N 0.8099(2) 0.04836(17) 0.28399(11) 0.0264(6) Uani 1 1 d . . . N5 N 0.8898(2) 0.16290(17) 0.16132(11) 0.0267(6) Uani 1 1 d . . . N6 N 1.0813(2) 0.12108(17) 0.14852(11) 0.0268(6) Uani 1 1 d . . . C1 C 1.4078(3) 0.1826(2) 0.29534(17) 0.0408(9) Uani 1 1 d . . . H1A H 1.4216 0.1747 0.2557 0.049 Uiso 1 1 calc R . . C2 C 1.4747(3) 0.2258(3) 0.3334(2) 0.0507(11) Uani 1 1 d . . . H2B H 1.5441 0.2525 0.3255 0.061 Uiso 1 1 calc R . . C3 C 1.4247(3) 0.2251(3) 0.3874(2) 0.0500(11) Uani 1 1 d . . . C4 C 1.4496(4) 0.2579(4) 0.4423(2) 0.0828(17) Uani 1 1 d . . . H4A H 1.5171 0.2890 0.4508 0.099 Uiso 1 1 calc R . . C5 C 1.3744(5) 0.2445(4) 0.4839(2) 0.101(2) Uani 1 1 d . . . H5A H 1.3893 0.2668 0.5218 0.121 Uiso 1 1 calc R . . C6 C 1.2763(4) 0.1981(4) 0.4709(2) 0.0771(15) Uani 1 1 d . . . H6A H 1.2254 0.1908 0.5006 0.092 Uiso 1 1 calc R . . C7 C 1.3239(3) 0.1771(2) 0.38017(17) 0.0406(9) Uani 1 1 d . . . C8 C 0.9932(3) -0.1002(2) 0.36038(14) 0.0356(8) Uani 1 1 d . . . H8A H 1.0642 -0.1222 0.3724 0.043 Uiso 1 1 calc R . . C9 C 0.8976(3) -0.1345(2) 0.37781(16) 0.0422(9) Uani 1 1 d . . . H9A H 0.8893 -0.1843 0.4036 0.051 Uiso 1 1 calc R . . C10 C 0.8092(3) -0.0819(2) 0.35016(14) 0.0346(8) Uani 1 1 d . . . C11 C 0.6953(3) -0.0813(3) 0.35024(17) 0.0476(10) Uani 1 1 d . . . H11A H 0.6558 -0.1249 0.3719 0.057 Uiso 1 1 calc R . . C12 C 0.6411(3) -0.0152(3) 0.31768(17) 0.0494(10) Uani 1 1 d . . . H12A H 0.5627 -0.0126 0.3172 0.059 Uiso 1 1 calc R . . C13 C 0.6987(3) 0.0477(2) 0.28553(15) 0.0365(8) Uani 1 1 d . . . H13A H 0.6580 0.0921 0.2637 0.044 Uiso 1 1 calc R . . C14 C 0.8607(3) -0.0164(2) 0.31617(13) 0.0277(7) Uani 1 1 d . . . C15 C 1.1489(3) 0.1169(2) 0.10159(15) 0.0345(8) Uani 1 1 d . . . H15A H 1.2251 0.1012 0.1035 0.041 Uiso 1 1 calc R . . C16 C 1.0901(3) 0.1384(2) 0.05296(15) 0.0353(8) Uani 1 1 d . . . H16A H 1.1174 0.1400 0.0152 0.042 Uiso 1 1 calc R . . C17 C 0.9796(3) 0.1582(2) 0.06844(13) 0.0293(7) Uani 1 1 d . . . C18 C 0.8819(3) 0.1858(2) 0.03990(15) 0.0389(9) Uani 1 1 d . . . H18A H 0.8785 0.1947 -0.0006 0.047 Uiso 1 1 calc R . . C19 C 0.7906(3) 0.2000(3) 0.07214(15) 0.0415(9) Uani 1 1 d . . . H19A H 0.7227 0.2180 0.0537 0.050 Uiso 1 1 calc R . . C20 C 0.7971(3) 0.1880(2) 0.13181(15) 0.0360(8) Uani 1 1 d . . . H20A H 0.7324 0.1981 0.1527 0.043 Uiso 1 1 calc R . . C21 C 0.9765(3) 0.14742(19) 0.12859(14) 0.0258(7) Uani 1 1 d . . . C22 C 1.1465(3) 0.0585(2) 0.32257(14) 0.0290(8) Uani 1 1 d . . . H22A H 1.1594 0.0457 0.3624 0.035 Uiso 1 1 calc R . . C23 C 1.2207(3) 0.1114(2) 0.29319(14) 0.0299(8) Uani 1 1 d . . . C24 C 1.2015(3) 0.1326(2) 0.23506(14) 0.0291(8) Uani 1 1 d . . . H24A H 1.2515 0.1703 0.2152 0.035 Uiso 1 1 calc R . . C25 C 1.1077(3) 0.0973(2) 0.20691(13) 0.0257(7) Uani 1 1 d . . . C26 C 1.0348(3) 0.0411(2) 0.23482(13) 0.0230(7) Uani 1 1 d . . . C27 C 1.0539(3) 0.02448(19) 0.29371(14) 0.0241(7) Uani 1 1 d . . . H26 H 0.980(3) 0.008(2) 0.2143(15) 0.050 Uiso 1 1 d . . . C28 C 0.7829(3) 0.3398(2) 0.31180(14) 0.0286(7) Uani 1 1 d . . . C29 C 0.7351(3) 0.3514(2) 0.25723(16) 0.0427(9) Uani 1 1 d . . . H29A H 0.7648 0.3198 0.2256 0.051 Uiso 1 1 calc R . . C30 C 0.6441(3) 0.4085(3) 0.24808(18) 0.0544(11) Uani 1 1 d . . . H30A H 0.6116 0.4150 0.2104 0.065 Uiso 1 1 calc R . . C31 C 0.6018(3) 0.4548(3) 0.29282(19) 0.0484(10) Uani 1 1 d . . . H31A H 0.5392 0.4932 0.2864 0.058 Uiso 1 1 calc R . . C32 C 0.6485(3) 0.4465(2) 0.34719(18) 0.0417(9) Uani 1 1 d . . . H32A H 0.6194 0.4801 0.3782 0.050 Uiso 1 1 calc R . . C33 C 0.7386(3) 0.3891(2) 0.35689(16) 0.0367(8) Uani 1 1 d . . . H33A H 0.7705 0.3832 0.3947 0.044 Uiso 1 1 calc R . . C34 C 1.0215(3) 0.32897(19) 0.33443(14) 0.0264(7) Uani 1 1 d . . . C35 C 1.1057(3) 0.3249(2) 0.29618(15) 0.0299(8) Uani 1 1 d . . . H35A H 1.0968 0.2889 0.2622 0.036 Uiso 1 1 calc R . . C36 C 1.2043(3) 0.3734(2) 0.30700(17) 0.0401(9) Uani 1 1 d . . . H36A H 1.2623 0.3691 0.2808 0.048 Uiso 1 1 calc R . . C37 C 1.2172(3) 0.4271(2) 0.35529(17) 0.0430(10) Uani 1 1 d . . . H37A H 1.2839 0.4601 0.3626 0.052 Uiso 1 1 calc R . . C38 C 1.1323(3) 0.4326(2) 0.39327(15) 0.0413(9) Uani 1 1 d . . . H38A H 1.1407 0.4704 0.4265 0.050 Uiso 1 1 calc R . . C39 C 1.0355(3) 0.3839(2) 0.38362(14) 0.0339(8) Uani 1 1 d . . . H39A H 0.9784 0.3877 0.4104 0.041 Uiso 1 1 calc R . . C40 C 0.8772(3) 0.2011(2) 0.38742(13) 0.0257(7) Uani 1 1 d . . . C41 C 0.7722(3) 0.1770(2) 0.40358(14) 0.0340(8) Uani 1 1 d . . . H41A H 0.7094 0.1987 0.3819 0.041 Uiso 1 1 calc R . . C42 C 0.7579(3) 0.1212(2) 0.45148(16) 0.0432(9) Uani 1 1 d . . . H42A H 0.6857 0.1055 0.4626 0.052 Uiso 1 1 calc R . . C43 C 0.8485(3) 0.0888(2) 0.48248(16) 0.0467(10) Uani 1 1 d . . . H43A H 0.8388 0.0504 0.5150 0.056 Uiso 1 1 calc R . . C44 C 0.9531(3) 0.1116(2) 0.46665(15) 0.0422(9) Uani 1 1 d . . . H44A H 1.0152 0.0889 0.4884 0.051 Uiso 1 1 calc R . . C45 C 0.9688(3) 0.1670(2) 0.41963(14) 0.0312(8) Uani 1 1 d . . . H45A H 1.0415 0.1822 0.4090 0.037 Uiso 1 1 calc R . . F1 F 0.5528(4) 0.1723(7) 0.1891(3) 0.082(2) Uani 0.60 1 d P . . F1A F 0.5381(5) 0.2165(7) 0.0862(3) 0.065(2) Uani 0.40 1 d P . . F2 F 0.5383(4) 0.2751(5) 0.1198(4) 0.0871(18) Uani 0.60 1 d P . . F2A F 0.5512(6) 0.1099(7) 0.1519(6) 0.097(3) Uani 0.40 1 d P . . F4 F 0.3887(2) 0.1958(2) 0.14504(14) 0.1057(12) Uani 1 1 d . . . F3A F 0.5073(8) 0.1325(6) 0.1009(4) 0.164(3) Uani 0.60 1 d P . . F3 F 0.5357(9) 0.2568(11) 0.1775(6) 0.142(5) Uani 0.40 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.043(3) 0.055(3) 0.044(3) -0.001(3) -0.007(2) -0.011(2) P1 0.0289(5) 0.0261(4) 0.0212(5) 0.0006(3) 0.0023(4) 0.0006(4) Cu1 0.0287(2) 0.0298(2) 0.0200(2) -0.00035(18) 0.00215(16) 0.00060(18) N1 0.0236(15) 0.0441(16) 0.0386(18) -0.0018(14) -0.0038(13) -0.0044(13) N2 0.041(2) 0.076(2) 0.039(2) -0.0164(18) -0.0045(16) -0.0002(18) N3 0.0309(16) 0.0272(13) 0.0261(15) 0.0049(12) -0.0008(12) -0.0013(12) N4 0.0231(15) 0.0343(14) 0.0219(15) -0.0010(12) 0.0008(12) -0.0021(12) N5 0.0272(15) 0.0341(14) 0.0189(14) 0.0009(12) 0.0024(12) 0.0011(12) N6 0.0288(15) 0.0294(13) 0.0225(15) 0.0021(12) 0.0064(12) 0.0027(12) C1 0.028(2) 0.043(2) 0.051(2) 0.0025(18) 0.0010(18) -0.0008(16) C2 0.029(2) 0.049(2) 0.073(3) -0.002(2) -0.010(2) -0.0065(18) C3 0.036(2) 0.053(2) 0.060(3) -0.015(2) -0.009(2) -0.0005(19) C4 0.059(3) 0.110(4) 0.078(4) -0.040(3) -0.014(3) -0.021(3) C5 0.087(4) 0.149(6) 0.064(4) -0.053(4) -0.017(3) -0.024(4) C6 0.064(3) 0.116(4) 0.051(3) -0.031(3) -0.005(3) -0.006(3) C7 0.032(2) 0.043(2) 0.045(2) -0.0105(18) -0.0103(19) 0.0036(17) C8 0.043(2) 0.0369(18) 0.0263(19) 0.0082(16) -0.0024(17) 0.0026(17) C9 0.053(3) 0.038(2) 0.035(2) 0.0115(17) 0.0049(19) -0.0048(18) C10 0.040(2) 0.0371(18) 0.0273(19) 0.0021(16) 0.0057(16) -0.0097(16) C11 0.044(2) 0.055(2) 0.045(2) 0.010(2) 0.0060(19) -0.018(2) C12 0.031(2) 0.069(3) 0.048(3) -0.001(2) 0.0030(19) -0.018(2) C13 0.033(2) 0.045(2) 0.032(2) -0.0036(17) -0.0008(16) -0.0028(16) C14 0.0293(19) 0.0329(17) 0.0208(18) -0.0052(14) -0.0007(14) -0.0053(15) C15 0.036(2) 0.0311(17) 0.038(2) -0.0003(16) 0.0132(17) 0.0037(16) C16 0.048(2) 0.0346(18) 0.0238(19) -0.0002(15) 0.0124(17) -0.0003(16) C17 0.041(2) 0.0311(16) 0.0165(16) 0.0006(14) 0.0060(15) 0.0011(16) C18 0.051(2) 0.048(2) 0.0178(18) 0.0035(16) -0.0009(17) -0.0002(18) C19 0.037(2) 0.061(2) 0.026(2) 0.0035(18) -0.0040(17) 0.0067(19) C20 0.030(2) 0.051(2) 0.0273(19) -0.0001(16) 0.0010(16) 0.0054(16) C21 0.0301(18) 0.0221(15) 0.0254(17) -0.0006(14) 0.0032(14) 0.0007(14) C22 0.0270(18) 0.0356(17) 0.0241(18) 0.0010(15) -0.0022(15) 0.0035(15) C23 0.0223(18) 0.0332(17) 0.034(2) -0.0050(15) 0.0009(15) 0.0030(15) C24 0.0215(17) 0.0345(17) 0.0317(19) 0.0004(15) 0.0059(15) 0.0023(14) C25 0.0273(18) 0.0273(16) 0.0230(17) -0.0040(14) 0.0074(14) 0.0050(14) C26 0.0228(17) 0.0236(15) 0.0226(17) -0.0024(13) -0.0004(14) 0.0022(13) C27 0.0237(17) 0.0212(14) 0.0276(18) -0.0008(13) 0.0041(14) 0.0022(13) C28 0.0282(18) 0.0232(15) 0.0345(19) -0.0011(15) 0.0025(15) 0.0014(14) C29 0.045(2) 0.048(2) 0.035(2) -0.0006(18) 0.0037(18) 0.0125(19) C30 0.052(3) 0.063(3) 0.047(3) 0.007(2) -0.009(2) 0.021(2) C31 0.036(2) 0.042(2) 0.067(3) 0.004(2) -0.001(2) 0.0090(18) C32 0.040(2) 0.0310(18) 0.055(3) -0.0092(18) 0.0113(19) 0.0016(17) C33 0.037(2) 0.0366(18) 0.037(2) -0.0040(17) 0.0018(17) 0.0005(16) C34 0.0288(18) 0.0235(15) 0.0269(18) 0.0050(14) 0.0002(15) 0.0002(14) C35 0.0311(19) 0.0287(17) 0.0296(18) 0.0034(15) -0.0001(15) 0.0026(15) C36 0.033(2) 0.0409(19) 0.047(2) 0.0116(18) 0.0061(18) 0.0031(16) C37 0.035(2) 0.044(2) 0.050(3) 0.0127(19) -0.0125(19) -0.0103(18) C38 0.056(3) 0.0367(19) 0.030(2) 0.0026(17) -0.0106(19) -0.0080(19) C39 0.043(2) 0.0346(17) 0.0237(19) 0.0026(15) 0.0040(16) -0.0034(16) C40 0.0296(19) 0.0270(16) 0.0206(17) -0.0026(13) 0.0039(14) -0.0014(14) C41 0.033(2) 0.0425(19) 0.0268(19) 0.0003(16) 0.0053(16) -0.0046(16) C42 0.044(2) 0.050(2) 0.037(2) 0.0007(18) 0.0096(19) -0.0136(18) C43 0.069(3) 0.042(2) 0.029(2) 0.0128(17) 0.007(2) -0.006(2) C44 0.058(3) 0.039(2) 0.029(2) 0.0057(17) -0.0010(19) 0.0070(19) C45 0.0321(19) 0.0327(17) 0.0292(19) -0.0013(15) 0.0049(15) 0.0051(15) F1 0.038(3) 0.155(6) 0.054(3) 0.051(4) 0.007(2) 0.023(4) F1A 0.033(3) 0.117(7) 0.044(4) 0.028(4) 0.005(3) -0.006(4) F2 0.054(3) 0.101(4) 0.106(5) 0.061(4) 0.003(4) -0.015(3) F2A 0.043(4) 0.101(7) 0.146(9) 0.089(7) 0.013(6) 0.006(4) F4 0.0312(15) 0.156(3) 0.129(3) 0.075(2) -0.0031(16) -0.0145(16) F3A 0.237(10) 0.130(6) 0.125(7) -0.055(6) 0.016(7) -0.038(6) F3 0.102(8) 0.202(12) 0.124(10) -0.106(10) 0.039(7) -0.083(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 F3 1.299(9) . ? B1 F3A 1.316(8) . ? B1 F1 1.330(7) . ? B1 F4 1.342(5) . ? B1 F2 1.343(7) . ? B1 F1A 1.398(8) . ? B1 F2A 1.429(9) . ? P1 C34 1.820(3) . ? P1 C28 1.822(3) . ? P1 C40 1.829(3) . ? P1 Cu1 2.2277(10) . ? Cu1 N5 2.022(3) . ? Cu1 N4 2.076(3) . ? Cu1 C26 2.429(3) . ? N1 C7 1.392(5) . ? N1 C1 1.394(5) . ? N1 C23 1.426(4) . ? N2 C7 1.313(5) . ? N2 C6 1.344(5) . ? N3 C14 1.386(4) . ? N3 C8 1.393(4) . ? N3 C27 1.413(4) . ? N4 C14 1.339(4) . ? N4 C13 1.350(4) . ? N5 C21 1.339(4) . ? N5 C20 1.343(4) . ? N6 C21 1.389(4) . ? N6 C15 1.390(4) . ? N6 C25 1.425(4) . ? C1 C2 1.334(5) . ? C2 C3 1.416(6) . ? C3 C4 1.383(6) . ? C3 C7 1.412(5) . ? C4 C5 1.368(7) . ? C5 C6 1.391(7) . ? C8 C9 1.338(5) . ? C9 C10 1.448(5) . ? C10 C11 1.380(5) . ? C10 C14 1.401(4) . ? C11 C12 1.376(5) . ? C12 C13 1.387(5) . ? C15 C16 1.349(5) . ? C16 C17 1.429(5) . ? C17 C18 1.395(5) . ? C17 C21 1.408(4) . ? C18 C19 1.375(5) . ? C19 C20 1.396(5) . ? C22 C27 1.378(4) . ? C22 C23 1.383(5) . ? C23 C24 1.396(4) . ? C24 C25 1.388(4) . ? C25 C26 1.384(4) . ? C26 C27 1.400(4) . ? C28 C29 1.384(5) . ? C28 C33 1.394(5) . ? C29 C30 1.390(5) . ? C30 C31 1.356(5) . ? C31 C32 1.370(5) . ? C32 C33 1.387(5) . ? C34 C35 1.380(5) . ? C34 C39 1.400(4) . ? C35 C36 1.403(5) . ? C36 C37 1.371(5) . ? C37 C38 1.383(5) . ? C38 C39 1.381(5) . ? C40 C41 1.385(4) . ? C40 C45 1.405(4) . ? C41 C42 1.395(5) . ? C42 C43 1.373(5) . ? C43 C44 1.373(5) . ? C44 C45 1.378(5) . ? F1 F2A 1.255(12) . ? F1 F3 1.276(15) . ? F1A F2 1.157(8) . ? F1A F3A 1.328(10) . ? F2 F3 1.369(14) . ? F2A F3A 1.322(11) . ? 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 F3 B1 F3A 155.4(8) . . ? F3 B1 F1 58.1(7) . . ? F3A B1 F1 111.2(6) . . ? F3 B1 F4 105.6(6) . . ? F3A B1 F4 99.0(5) . . ? F1 B1 F4 113.1(5) . . ? F3 B1 F2 62.4(7) . . ? F3A B1 F2 108.3(6) . . ? F1 B1 F2 111.0(5) . . ? F4 B1 F2 113.6(4) . . ? F3 B1 F1A 109.4(8) . . ? F3A B1 F1A 58.5(5) . . ? F1 B1 F1A 130.4(5) . . ? F4 B1 F1A 116.4(4) . . ? F2 B1 F1A 49.9(4) . . ? F3 B1 F2A 109.7(9) . . ? F3A B1 F2A 57.4(6) . . ? F1 B1 F2A 54.0(5) . . ? F4 B1 F2A 114.7(5) . . ? F2 B1 F2A 131.2(5) . . ? F1A B1 F2A 100.9(7) . . ? C34 P1 C28 106.68(14) . . ? C34 P1 C40 103.49(14) . . ? C28 P1 C40 104.44(15) . . ? C34 P1 Cu1 120.67(11) . . ? C28 P1 Cu1 111.31(11) . . ? C40 P1 Cu1 108.87(10) . . ? N5 Cu1 N4 115.82(10) . . ? N5 Cu1 P1 135.30(8) . . ? N4 Cu1 P1 102.54(8) . . ? N5 Cu1 C26 83.78(10) . . ? N4 Cu1 C26 82.94(11) . . ? P1 Cu1 C26 124.64(8) . . ? C7 N1 C1 107.9(3) . . ? C7 N1 C23 127.2(3) . . ? C1 N1 C23 124.2(3) . . ? C7 N2 C6 113.9(4) . . ? C14 N3 C8 107.1(3) . . ? C14 N3 C27 125.5(3) . . ? C8 N3 C27 127.4(3) . . ? C14 N4 C13 114.7(3) . . ? C14 N4 Cu1 122.6(2) . . ? C13 N4 Cu1 121.6(2) . . ? C21 N5 C20 114.5(3) . . ? C21 N5 Cu1 124.7(2) . . ? C20 N5 Cu1 120.8(2) . . ? C21 N6 C15 108.0(3) . . ? C21 N6 C25 123.7(3) . . ? C15 N6 C25 128.2(3) . . ? C2 C1 N1 109.8(4) . . ? C1 C2 C3 108.3(4) . . ? C4 C3 C7 116.0(4) . . ? C4 C3 C2 136.8(4) . . ? C7 C3 C2 107.2(3) . . ? C5 C4 C3 118.3(4) . . ? C4 C5 C6 120.1(5) . . ? N2 C6 C5 123.9(5) . . ? N2 C7 N1 125.5(3) . . ? N2 C7 C3 127.7(4) . . ? N1 C7 C3 106.8(4) . . ? C9 C8 N3 110.6(3) . . ? C8 C9 C10 107.6(3) . . ? C11 C10 C14 117.7(3) . . ? C11 C10 C9 136.5(3) . . ? C14 C10 C9 105.8(3) . . ? C12 C11 C10 117.3(3) . . ? C11 C12 C13 121.3(4) . . ? N4 C13 C12 122.8(3) . . ? N4 C14 N3 125.0(3) . . ? N4 C14 C10 126.1(3) . . ? N3 C14 C10 108.9(3) . . ? C16 C15 N6 109.8(3) . . ? C15 C16 C17 107.8(3) . . ? C18 C17 C21 116.7(3) . . ? C18 C17 C16 136.5(3) . . ? C21 C17 C16 106.8(3) . . ? C19 C18 C17 118.1(3) . . ? C18 C19 C20 120.4(3) . . ? N5 C20 C19 123.7(3) . . ? N5 C21 N6 125.7(3) . . ? N5 C21 C17 126.6(3) . . ? N6 C21 C17 107.6(3) . . ? C27 C22 C23 119.5(3) . . ? C22 C23 C24 120.9(3) . . ? C22 C23 N1 120.7(3) . . ? C24 C23 N1 118.3(3) . . ? C25 C24 C23 118.5(3) . . ? C26 C25 C24 121.6(3) . . ? C26 C25 N6 117.8(3) . . ? C24 C25 N6 120.6(3) . . ? C25 C26 C27 118.4(3) . . ? C25 C26 Cu1 96.38(19) . . ? C27 C26 Cu1 94.86(19) . . ? C22 C27 C26 121.0(3) . . ? C22 C27 N3 121.6(3) . . ? C26 C27 N3 117.5(3) . . ? C29 C28 C33 117.7(3) . . ? C29 C28 P1 117.3(3) . . ? C33 C28 P1 125.0(3) . . ? C28 C29 C30 121.0(4) . . ? C31 C30 C29 120.1(4) . . ? C30 C31 C32 120.5(3) . . ? C31 C32 C33 119.9(4) . . ? C32 C33 C28 120.8(3) . . ? C35 C34 C39 118.7(3) . . ? C35 C34 P1 118.2(2) . . ? C39 C34 P1 123.1(3) . . ? C34 C35 C36 120.6(3) . . ? C37 C36 C35 120.3(4) . . ? C36 C37 C38 119.4(3) . . ? C39 C38 C37 120.9(3) . . ? C38 C39 C34 120.2(3) . . ? C41 C40 C45 118.7(3) . . ? C41 C40 P1 121.0(2) . . ? C45 C40 P1 119.5(2) . . ? C40 C41 C42 120.5(3) . . ? C43 C42 C41 119.9(4) . . ? C42 C43 C44 120.2(3) . . ? C43 C44 C45 120.7(3) . . ? C44 C45 C40 120.0(3) . . ? F2A F1 F3 123.7(8) . . ? F2A F1 B1 67.0(5) . . ? F3 F1 B1 59.8(5) . . ? F2 F1A F3A 120.1(7) . . ? F2 F1A B1 62.6(5) . . ? F3A F1A B1 57.7(5) . . ? F1A F2 B1 67.5(5) . . ? F1A F2 F3 121.1(9) . . ? B1 F2 F3 57.2(5) . . ? F1 F2A F3A 115.7(8) . . ? F1 F2A B1 59.0(6) . . ? F3A F2A B1 57.0(4) . . ? B1 F3A F2A 65.6(6) . . ? B1 F3A F1A 63.8(5) . . ? F2A F3A F1A 110.6(7) . . ? F1 F3 B1 62.1(6) . . ? F1 F3 F2 112.7(8) . . ? B1 F3 F2 60.4(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.591 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.070 #_Squeeze_results loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.500 0.500 100.2 35.1 2 0.500 1.000 0.000 100.2 34.9 3 0.500 0.500 1.000 119.8 36.2 4 0.500 1.000 0.500 119.8 36.0 _platon_squeeze_details ; One CH2Cl2 molecule per molecule of 2 was removed. ; # Attachment '3.cif' data_jli6 _database_code_depnum_ccdc_archive 'CCDC 699118' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H50 B Cu F4 N9 O P' _chemical_formula_weight 1070.39 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.25700(10) _cell_length_b 15.4097(2) _cell_length_c 15.5266(2) _cell_angle_alpha 81.5200(10) _cell_angle_beta 85.3200(10) _cell_angle_gamma 69.1880(10) _cell_volume 2488.85(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9916 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 27.13 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8576 _exptl_absorpt_correction_T_max 0.9196 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23805 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.15 _reflns_number_total 10992 _reflns_number_gt 9210 _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^)+(0.0650P)^2^+0.9200P] 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 10992 _refine_ls_number_parameters 664 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1122 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Cu1 Cu -0.53720(2) 0.215096(15) 0.300002(15) 0.02448(8) Uani 1 1 d . . . B1 B -0.9557(3) 0.4911(2) 0.6960(2) 0.0460(6) Uani 1 1 d . . . P1 P -0.49681(5) 0.24789(3) 0.16021(3) 0.02616(12) Uani 1 1 d . . . N1 N -0.65873(14) 0.14205(11) 0.34383(10) 0.0239(3) Uani 1 1 d . . . N2 N -0.55027(16) 0.30560(11) 0.38863(11) 0.0287(3) Uani 1 1 d . . . N3 N -0.49278(14) -0.00403(10) 0.36494(11) 0.0246(3) Uani 1 1 d . . . N4 N -0.08851(14) 0.00672(11) 0.23906(10) 0.0253(3) Uani 1 1 d . . . N5 N -0.33816(15) 0.23369(11) 0.43283(11) 0.0275(3) Uani 1 1 d . . . N6 N -0.51215(18) -0.11468(13) 0.28322(13) 0.0369(4) Uani 1 1 d . . . N7 N -0.08126(16) -0.14999(12) 0.24904(13) 0.0353(4) Uani 1 1 d . . . N8 N -0.17298(19) 0.17027(13) 0.53100(12) 0.0375(4) Uani 1 1 d . . . N9 N 0.12228(17) 0.00859(14) 0.21819(12) 0.0364(4) Uani 1 1 d . . . C1 C -0.45351(18) -0.09860(13) 0.34656(14) 0.0279(4) Uani 1 1 d . . . C2 C -0.3532(2) -0.16655(14) 0.39233(16) 0.0370(5) Uani 1 1 d . . . H2A H -0.3167 -0.1522 0.4390 0.044 Uiso 1 1 calc R . . C3 C -0.3089(2) -0.25509(16) 0.3677(2) 0.0507(7) Uani 1 1 d . . . H3A H -0.2393 -0.3030 0.3961 0.061 Uiso 1 1 calc R . . C4 C -0.3670(3) -0.27311(17) 0.3010(2) 0.0595(8) Uani 1 1 d . . . H4A H -0.3372 -0.3333 0.2821 0.071 Uiso 1 1 calc R . . C5 C -0.4691(3) -0.20237(18) 0.2624(2) 0.0527(7) Uani 1 1 d . . . H5A H -0.5113 -0.2164 0.2186 0.063 Uiso 1 1 calc R . . C6 C -0.6670(2) 0.37271(14) 0.39710(16) 0.0371(5) Uani 1 1 d . . . H6B H -0.7316 0.3769 0.3593 0.045 Uiso 1 1 calc R . . C7 C -0.6960(2) 0.43445(16) 0.45740(19) 0.0467(6) Uani 1 1 d . . . H7B H -0.7781 0.4810 0.4605 0.056 Uiso 1 1 calc R . . C8 C -0.6032(2) 0.42742(16) 0.51333(18) 0.0464(6) Uani 1 1 d . . . H8B H -0.6212 0.4686 0.5564 0.056 Uiso 1 1 calc R . . C9 C -0.4839(2) 0.36019(16) 0.50646(15) 0.0382(5) Uani 1 1 d . . . H9B H -0.4191 0.3545 0.5447 0.046 Uiso 1 1 calc R . . C10 C -0.45988(19) 0.30053(13) 0.44232(13) 0.0286(4) Uani 1 1 d . . . C11 C -0.06360(17) -0.07622(13) 0.19984(13) 0.0256(4) Uani 1 1 d . . . C12 C -0.0215(2) -0.07612(16) 0.11383(14) 0.0345(4) Uani 1 1 d . . . H12A H -0.0105 -0.0221 0.0813 0.041 Uiso 1 1 calc R . . C13 C 0.00400(17) -0.15697(15) 0.07675(13) 0.0515(6) Uani 1 1 d . . . H13A H 0.0345 -0.1597 0.0180 0.062 Uiso 1 1 calc R . . C14 C -0.01480(17) -0.23393(15) 0.12493(13) 0.0537(7) Uani 1 1 d R . . H14A H 0.0015 -0.2904 0.0996 0.064 Uiso 1 1 d R . . C15 C -0.0576(2) -0.22758(16) 0.2105(2) 0.0475(6) Uani 1 1 d . . . H15A H -0.0711 -0.2804 0.2438 0.057 Uiso 1 1 calc R . . C16 C -0.78462(18) 0.19223(14) 0.34954(13) 0.0292(4) Uani 1 1 d . . . H16A H -0.8118 0.2575 0.3304 0.035 Uiso 1 1 calc R . . C17 C -0.87502(19) 0.15433(15) 0.38123(14) 0.0325(4) Uani 1 1 d . . . H17A H -0.9623 0.1923 0.3842 0.039 Uiso 1 1 calc R . . C18 C -0.83555(18) 0.05870(15) 0.40895(13) 0.0310(4) Uani 1 1 d . . . H18A H -0.8959 0.0304 0.4316 0.037 Uiso 1 1 calc R . . C19 C -0.70975(18) 0.00590(14) 0.40338(12) 0.0262(4) Uani 1 1 d . . . H19A H -0.6817 -0.0596 0.4217 0.031 Uiso 1 1 calc R . . C20 C -0.62203(17) 0.04936(13) 0.37027(12) 0.0224(4) Uani 1 1 d . . . C21 C -0.23251(18) 0.24151(14) 0.47240(13) 0.0277(4) Uani 1 1 d . . . C22 C -0.1983(2) 0.31995(14) 0.44902(15) 0.0330(4) Uani 1 1 d . . . H22A H -0.2406 0.3676 0.4044 0.040 Uiso 1 1 calc R . . C23 C -0.0992(2) 0.32640(16) 0.49359(16) 0.0388(5) Uani 1 1 d . . . H23A H -0.0737 0.3795 0.4807 0.047 Uiso 1 1 calc R . . C24 C -0.0398(2) 0.25480(18) 0.55595(16) 0.0426(5) Uani 1 1 d . . . H24A H 0.0260 0.2582 0.5884 0.051 Uiso 1 1 calc R . . C25 C -0.0768(3) 0.17761(18) 0.57101(16) 0.0467(6) Uani 1 1 d . . . H25A H -0.0315 0.1268 0.6121 0.056 Uiso 1 1 calc R . . C26 C -0.00490(17) 0.05742(13) 0.21162(12) 0.0247(4) Uani 1 1 d . . . C27 C -0.05432(18) 0.14831(13) 0.17864(12) 0.0261(4) Uani 1 1 d . . . H27A H -0.1436 0.1795 0.1746 0.031 Uiso 1 1 calc R . . C28 C 0.0287(2) 0.19397(16) 0.15123(14) 0.0400(5) Uani 1 1 d . . . H28A H -0.0037 0.2584 0.1288 0.048 Uiso 1 1 calc R . . C29 C 0.1578(2) 0.14889(17) 0.15526(14) 0.0386(5) Uani 1 1 d . . . H29A H 0.2146 0.1813 0.1356 0.046 Uiso 1 1 calc R . . C30 C 0.2032(2) 0.05553(17) 0.18846(14) 0.0366(5) Uani 1 1 d . . . H30A H 0.2924 0.0232 0.1907 0.044 Uiso 1 1 calc R . . C31 C -0.20953(17) 0.11763(12) 0.33973(12) 0.0226(4) Uani 1 1 d . . . H31A H -0.1454 0.1450 0.3347 0.027 Uiso 1 1 calc R . . C32 C -0.19564(16) 0.04232(12) 0.29433(11) 0.0214(3) Uani 1 1 d . . . C33 C -0.29321(16) 0.00564(12) 0.29999(12) 0.0222(4) Uani 1 1 d . . . H33A H -0.2885 -0.0413 0.2652 0.027 Uiso 1 1 calc R . . C34 C -0.39744(16) 0.03756(12) 0.35639(12) 0.0210(3) Uani 1 1 d . . . C35 C -0.40933(16) 0.10924(12) 0.40543(11) 0.0219(3) Uani 1 1 d . . . H35A H -0.4477 0.1046 0.4656 0.026 Uiso 1 1 calc R . . C36 C -0.31781(17) 0.15216(12) 0.39222(12) 0.0225(4) Uani 1 1 d . . . C37 C -0.40282(19) 0.32405(15) 0.13256(15) 0.0344(5) Uani 1 1 d . . . C38 C -0.3344(2) 0.33492(16) 0.19828(17) 0.0404(5) Uani 1 1 d . . . H38A H -0.3394 0.3043 0.2555 0.049 Uiso 1 1 calc R . . C39 C -0.2588(2) 0.39033(18) 0.1809(2) 0.0528(7) Uani 1 1 d . . . H39A H -0.2125 0.3977 0.2261 0.063 Uiso 1 1 calc R . . C40 C -0.2514(3) 0.4343(2) 0.0982(2) 0.0642(9) Uani 1 1 d . . . H40A H -0.1988 0.4713 0.0861 0.077 Uiso 1 1 calc R . . C41 C -0.3195(3) 0.4252(2) 0.0327(2) 0.0679(9) Uani 1 1 d . . . H41A H -0.3144 0.4567 -0.0241 0.082 Uiso 1 1 calc R . . C42 C -0.3962(2) 0.37000(19) 0.04893(17) 0.0508(6) Uani 1 1 d . . . H42A H -0.4432 0.3639 0.0035 0.061 Uiso 1 1 calc R . . C43 C -0.63983(18) 0.30359(14) 0.09610(13) 0.0289(4) Uani 1 1 d . . . C44 C -0.74828(19) 0.36278(14) 0.13548(14) 0.0324(4) Uani 1 1 d . . . H44A H -0.7442 0.3764 0.1926 0.039 Uiso 1 1 calc R . . C45 C -0.8623(2) 0.40211(15) 0.09207(16) 0.0382(5) Uani 1 1 d . . . H45A H -0.9357 0.4422 0.1195 0.046 Uiso 1 1 calc R . . C46 C -0.8681(2) 0.38245(15) 0.00862(15) 0.0381(5) Uani 1 1 d . . . H46A H -0.9460 0.4085 -0.0210 0.046 Uiso 1 1 calc R . . C47 C -0.7615(2) 0.32541(16) -0.03163(15) 0.0402(5) Uani 1 1 d . . . H47A H -0.7656 0.3130 -0.0892 0.048 Uiso 1 1 calc R . . C48 C -0.6476(2) 0.28587(16) 0.01184(14) 0.0352(5) Uani 1 1 d . . . H48A H -0.5744 0.2464 -0.0163 0.042 Uiso 1 1 calc R . . C49 C -0.41689(18) 0.14436(14) 0.10633(13) 0.0288(4) Uani 1 1 d . . . C50 C -0.4591(2) 0.06906(15) 0.13043(13) 0.0323(4) Uani 1 1 d . . . H50A H -0.5222 0.0727 0.1756 0.039 Uiso 1 1 calc R . . C51 C -0.4104(2) -0.01059(17) 0.08964(14) 0.0393(5) Uani 1 1 d . . . H51A H -0.4402 -0.0613 0.1065 0.047 Uiso 1 1 calc R . . C52 C -0.3181(2) -0.01648(19) 0.02403(17) 0.0475(6) Uani 1 1 d . . . H52A H -0.2842 -0.0712 -0.0042 0.057 Uiso 1 1 calc R . . C53 C -0.2757(2) 0.0572(2) -0.00010(18) 0.0551(7) Uani 1 1 d . . . H53A H -0.2126 0.0530 -0.0454 0.066 Uiso 1 1 calc R . . C54 C -0.3233(2) 0.13778(18) 0.04055(15) 0.0429(5) Uani 1 1 d . . . H54A H -0.2924 0.1879 0.0237 0.051 Uiso 1 1 calc R . . F1 F -0.9828(6) 0.4333(5) 0.6416(4) 0.0625(12) Uani 0.50 1 d P . . F1A F -0.9984(15) 0.4564(8) 0.6485(10) 0.227(7) Uani 0.50 1 d P . . F2 F -0.8544(11) 0.4909(9) 0.6652(10) 0.157(5) Uani 0.50 1 d P . . F2A F -0.8332(7) 0.4968(5) 0.6608(4) 0.0520(11) Uani 0.50 1 d P . . F3 F -0.9277(11) 0.4493(8) 0.7801(7) 0.083(3) Uani 0.50 1 d P . . F3A F -0.9457(11) 0.4433(7) 0.7756(6) 0.081(3) Uani 0.50 1 d P . . F4 F -1.0486(10) 0.5758(10) 0.6882(10) 0.060(2) Uani 0.50 1 d P . . F4A F -1.0247(12) 0.5865(10) 0.7021(10) 0.088(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02280(13) 0.02253(12) 0.02591(13) 0.00026(9) 0.00279(9) -0.00727(9) B1 0.0454(16) 0.0353(14) 0.0532(17) -0.0032(12) 0.0028(13) -0.0110(12) P1 0.0228(2) 0.0283(2) 0.0264(2) 0.00364(19) 0.00114(18) -0.0109(2) N1 0.0205(7) 0.0216(7) 0.0277(8) -0.0020(6) 0.0028(6) -0.0064(6) N2 0.0269(8) 0.0209(8) 0.0360(9) -0.0042(7) 0.0045(7) -0.0064(6) N3 0.0181(7) 0.0200(7) 0.0354(9) -0.0027(6) 0.0032(6) -0.0075(6) N4 0.0204(7) 0.0248(8) 0.0320(8) -0.0074(6) 0.0062(6) -0.0097(6) N5 0.0253(8) 0.0266(8) 0.0330(9) -0.0115(7) 0.0030(7) -0.0099(7) N6 0.0372(10) 0.0308(9) 0.0469(11) -0.0108(8) 0.0048(8) -0.0160(8) N7 0.0270(9) 0.0259(8) 0.0520(11) -0.0073(8) 0.0052(8) -0.0086(7) N8 0.0497(11) 0.0387(10) 0.0310(9) -0.0006(8) -0.0064(8) -0.0241(9) N9 0.0303(9) 0.0459(11) 0.0351(9) -0.0102(8) 0.0036(7) -0.0148(8) C1 0.0217(9) 0.0210(9) 0.0411(11) -0.0022(8) 0.0076(8) -0.0101(7) C2 0.0269(10) 0.0261(10) 0.0534(13) 0.0048(9) 0.0045(9) -0.0090(8) C3 0.0339(12) 0.0249(11) 0.085(2) 0.0050(12) 0.0125(12) -0.0074(9) C4 0.0574(17) 0.0259(12) 0.096(2) -0.0178(13) 0.0277(16) -0.0175(12) C5 0.0578(16) 0.0422(14) 0.0693(18) -0.0239(13) 0.0118(13) -0.0273(13) C6 0.0300(11) 0.0234(10) 0.0532(13) -0.0047(9) 0.0046(9) -0.0047(8) C7 0.0339(12) 0.0293(11) 0.0727(17) -0.0174(11) 0.0144(11) -0.0050(9) C8 0.0443(13) 0.0355(12) 0.0654(16) -0.0271(11) 0.0226(12) -0.0183(10) C9 0.0370(12) 0.0383(12) 0.0455(12) -0.0203(10) 0.0141(9) -0.0183(10) C10 0.0297(10) 0.0221(9) 0.0352(10) -0.0064(8) 0.0086(8) -0.0114(8) C11 0.0168(8) 0.0271(9) 0.0335(10) -0.0090(8) 0.0020(7) -0.0068(7) C12 0.0330(11) 0.0423(12) 0.0286(10) -0.0103(9) 0.0014(8) -0.0117(9) C13 0.0454(14) 0.0691(18) 0.0407(13) -0.0304(13) 0.0041(11) -0.0128(13) C14 0.0364(13) 0.0505(15) 0.082(2) -0.0412(15) 0.0006(12) -0.0123(11) C15 0.0313(12) 0.0313(11) 0.0809(19) -0.0150(12) 0.0078(12) -0.0111(9) C16 0.0240(9) 0.0250(9) 0.0352(10) -0.0051(8) 0.0017(8) -0.0046(8) C17 0.0190(9) 0.0372(11) 0.0386(11) -0.0108(9) 0.0042(8) -0.0052(8) C18 0.0238(9) 0.0404(11) 0.0319(10) -0.0043(9) 0.0065(8) -0.0167(9) C19 0.0237(9) 0.0280(9) 0.0271(9) 0.0004(7) 0.0016(7) -0.0116(8) C20 0.0197(8) 0.0245(9) 0.0229(8) -0.0022(7) 0.0018(7) -0.0083(7) C21 0.0285(10) 0.0272(9) 0.0301(10) -0.0105(8) 0.0052(8) -0.0117(8) C22 0.0327(11) 0.0245(9) 0.0429(12) -0.0087(8) 0.0085(9) -0.0118(8) C23 0.0368(12) 0.0341(11) 0.0535(14) -0.0194(10) 0.0136(10) -0.0201(10) C24 0.0400(12) 0.0522(14) 0.0441(13) -0.0181(11) -0.0015(10) -0.0218(11) C25 0.0559(15) 0.0489(14) 0.0407(13) -0.0016(11) -0.0131(11) -0.0239(12) C26 0.0227(9) 0.0305(10) 0.0245(9) -0.0063(7) 0.0045(7) -0.0137(8) C27 0.0208(9) 0.0268(9) 0.0296(9) -0.0025(8) 0.0034(7) -0.0083(7) C28 0.0495(14) 0.0368(12) 0.0354(11) -0.0008(9) 0.0070(10) -0.0204(10) C29 0.0409(12) 0.0512(13) 0.0354(11) -0.0094(10) 0.0117(9) -0.0316(11) C30 0.0242(10) 0.0542(14) 0.0358(11) -0.0138(10) 0.0036(8) -0.0168(10) C31 0.0192(8) 0.0233(9) 0.0269(9) -0.0036(7) 0.0010(7) -0.0098(7) C32 0.0170(8) 0.0214(8) 0.0241(9) -0.0014(7) 0.0007(6) -0.0053(7) C33 0.0189(8) 0.0197(8) 0.0281(9) -0.0036(7) 0.0004(7) -0.0068(7) C34 0.0158(8) 0.0186(8) 0.0271(9) 0.0014(7) -0.0011(6) -0.0057(7) C35 0.0203(8) 0.0221(8) 0.0216(8) -0.0006(7) 0.0023(6) -0.0068(7) C36 0.0239(9) 0.0204(8) 0.0227(8) -0.0021(7) -0.0013(7) -0.0072(7) C37 0.0265(10) 0.0310(10) 0.0430(12) 0.0087(9) 0.0005(8) -0.0125(8) C38 0.0349(12) 0.0334(11) 0.0529(14) 0.0080(10) -0.0065(10) -0.0159(9) C39 0.0385(13) 0.0433(13) 0.0797(19) 0.0077(13) -0.0095(12) -0.0225(11) C40 0.0441(15) 0.0518(16) 0.098(2) 0.0244(16) -0.0054(15) -0.0309(13) C41 0.0612(18) 0.0674(19) 0.072(2) 0.0342(16) 0.0008(15) -0.0364(16) C42 0.0472(14) 0.0568(15) 0.0490(14) 0.0191(12) -0.0021(11) -0.0289(12) C43 0.0256(9) 0.0301(10) 0.0294(10) 0.0059(8) -0.0011(8) -0.0118(8) C44 0.0308(10) 0.0287(10) 0.0341(11) 0.0019(8) 0.0003(8) -0.0087(8) C45 0.0303(11) 0.0268(10) 0.0494(13) 0.0046(9) -0.0007(9) -0.0040(8) C46 0.0312(11) 0.0339(11) 0.0457(13) 0.0080(9) -0.0110(9) -0.0101(9) C47 0.0423(13) 0.0423(12) 0.0350(11) 0.0041(10) -0.0094(9) -0.0154(10) C48 0.0297(11) 0.0395(12) 0.0315(11) -0.0009(9) 0.0009(8) -0.0082(9) C49 0.0214(9) 0.0351(10) 0.0263(9) -0.0006(8) -0.0008(7) -0.0066(8) C50 0.0321(10) 0.0368(11) 0.0273(10) -0.0026(8) 0.0018(8) -0.0121(9) C51 0.0428(13) 0.0400(12) 0.0341(11) -0.0059(9) -0.0061(9) -0.0119(10) C52 0.0385(13) 0.0540(15) 0.0456(14) -0.0219(12) 0.0019(10) -0.0053(11) C53 0.0374(13) 0.0772(19) 0.0499(15) -0.0240(14) 0.0184(11) -0.0170(13) C54 0.0330(12) 0.0548(14) 0.0412(12) -0.0067(11) 0.0113(9) -0.0179(11) F1 0.075(3) 0.051(2) 0.069(3) -0.027(2) -0.013(2) -0.0203(19) F1A 0.313(15) 0.100(8) 0.280(14) -0.003(7) -0.196(12) -0.052(8) F2 0.077(6) 0.106(7) 0.236(10) 0.022(6) 0.070(6) -0.003(4) F2A 0.034(2) 0.041(2) 0.078(3) 0.0008(19) 0.0165(19) -0.0162(19) F3 0.092(4) 0.063(6) 0.064(5) 0.002(4) -0.032(4) 0.013(4) F3A 0.141(8) 0.034(3) 0.056(5) 0.000(3) 0.035(4) -0.026(4) F4 0.036(2) 0.043(3) 0.078(5) -0.007(3) 0.000(2) 0.0122(19) F4A 0.107(8) 0.046(4) 0.069(5) 0.007(3) 0.013(5) 0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.0610(17) . ? Cu1 N1 2.0779(15) . ? Cu1 P1 2.2027(5) . ? Cu1 C35 2.3110(18) . ? B1 F1A 1.192(12) . ? B1 F2 1.200(11) . ? B1 F3A 1.333(9) . ? B1 F4 1.348(13) . ? B1 F3 1.376(10) . ? B1 F4A 1.411(15) . ? B1 F1 1.434(7) . ? B1 F2A 1.469(7) . ? P1 C49 1.818(2) . ? P1 C37 1.828(2) . ? P1 C43 1.830(2) . ? N1 C20 1.347(2) . ? N1 C16 1.355(2) . ? N2 C10 1.341(3) . ? N2 C6 1.364(3) . ? N3 C20 1.397(2) . ? N3 C34 1.421(2) . ? N3 C1 1.430(2) . ? N4 C32 1.411(2) . ? N4 C11 1.425(2) . ? N4 C26 1.427(2) . ? N5 C10 1.403(2) . ? N5 C36 1.426(2) . ? N5 C21 1.432(2) . ? N6 C1 1.326(3) . ? N6 C5 1.343(3) . ? N7 C11 1.340(3) . ? N7 C15 1.348(3) . ? N8 C21 1.328(3) . ? N8 C25 1.337(3) . ? N9 C26 1.365(3) . ? N9 C30 1.367(3) . ? C1 C2 1.396(3) . ? C2 C3 1.377(3) . ? C3 C4 1.379(4) . ? C4 C5 1.378(4) . ? C6 C7 1.371(3) . ? C7 C8 1.377(4) . ? C8 C9 1.382(3) . ? C9 C10 1.400(3) . ? C11 C12 1.380(3) . ? C12 C13 1.377(3) . ? C13 C14 1.3790 . ? C14 C15 1.381(3) . ? C16 C17 1.369(3) . ? C17 C18 1.390(3) . ? C18 C19 1.363(3) . ? C19 C20 1.405(2) . ? C21 C22 1.385(3) . ? C22 C23 1.400(3) . ? C23 C24 1.367(3) . ? C24 C25 1.377(3) . ? C26 C27 1.347(3) . ? C27 C28 1.365(3) . ? C28 C29 1.372(3) . ? C29 C30 1.378(3) . ? C31 C36 1.392(3) . ? C31 C32 1.401(3) . ? C32 C33 1.394(2) . ? C33 C34 1.391(2) . ? C34 C35 1.394(3) . ? C35 C36 1.397(2) . ? C37 C38 1.390(3) . ? C37 C42 1.394(3) . ? C38 C39 1.392(3) . ? C39 C40 1.372(4) . ? C40 C41 1.373(5) . ? C41 C42 1.399(4) . ? C43 C48 1.391(3) . ? C43 C44 1.396(3) . ? C44 C45 1.392(3) . ? C45 C46 1.385(3) . ? C46 C47 1.376(3) . ? C47 C48 1.391(3) . ? C49 C54 1.394(3) . ? C49 C50 1.395(3) . ? C50 C51 1.379(3) . ? C51 C52 1.383(3) . ? C52 C53 1.374(4) . ? C53 C54 1.389(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 N2 Cu1 N1 107.69(6) . . ? N2 Cu1 P1 122.17(5) . . ? N1 Cu1 P1 121.87(5) . . ? N2 Cu1 C35 81.40(6) . . ? N1 Cu1 C35 82.11(6) . . ? P1 Cu1 C35 130.08(5) . . ? F1A B1 F2 107.2(11) . . ? F1A B1 F3A 109.9(9) . . ? F2 B1 F3A 111.9(9) . . ? F1A B1 F4 97.0(8) . . ? F2 B1 F4 114.5(9) . . ? F3A B1 F4 115.0(9) . . ? F1A B1 F3 120.2(9) . . ? F2 B1 F3 103.0(9) . . ? F3A B1 F3 11.3(10) . . ? F4 B1 F3 115.4(9) . . ? F1A B1 F4A 115.0(8) . . ? F2 B1 F4A 103.8(8) . . ? F3A B1 F4A 109.0(8) . . ? F4 B1 F4A 18.4(9) . . ? F3 B1 F4A 105.9(8) . . ? F1A B1 F1 11.9(8) . . ? F2 B1 F1 100.2(8) . . ? F3A B1 F1 104.7(6) . . ? F4 B1 F1 108.8(6) . . ? F3 B1 F1 114.0(6) . . ? F4A B1 F1 126.8(6) . . ? F1A B1 F2A 110.5(10) . . ? F2 B1 F2A 3.9(9) . . ? F3A B1 F2A 112.0(6) . . ? F4 B1 F2A 111.6(7) . . ? F3 B1 F2A 102.5(6) . . ? F4A B1 F2A 100.2(6) . . ? F1 B1 F2A 103.8(4) . . ? C49 P1 C37 106.32(10) . . ? C49 P1 C43 100.97(9) . . ? C37 P1 C43 105.14(9) . . ? C49 P1 Cu1 113.24(6) . . ? C37 P1 Cu1 116.15(8) . . ? C43 P1 Cu1 113.56(6) . . ? C20 N1 C16 117.30(15) . . ? C20 N1 Cu1 125.27(12) . . ? C16 N1 Cu1 117.37(12) . . ? C10 N2 C6 117.72(18) . . ? C10 N2 Cu1 126.82(13) . . ? C6 N2 Cu1 115.25(15) . . ? C20 N3 C34 121.87(15) . . ? C20 N3 C1 120.01(15) . . ? C34 N3 C1 116.43(14) . . ? C32 N4 C11 122.86(15) . . ? C32 N4 C26 121.46(15) . . ? C11 N4 C26 115.37(14) . . ? C10 N5 C36 121.82(16) . . ? C10 N5 C21 119.75(16) . . ? C36 N5 C21 118.12(15) . . ? C1 N6 C5 116.5(2) . . ? C11 N7 C15 116.9(2) . . ? C21 N8 C25 116.77(19) . . ? C26 N9 C30 117.23(19) . . ? N6 C1 C2 124.25(19) . . ? N6 C1 N3 116.79(17) . . ? C2 C1 N3 118.87(19) . . ? C3 C2 C1 117.8(2) . . ? C2 C3 C4 119.0(2) . . ? C5 C4 C3 118.9(2) . . ? N6 C5 C4 123.5(3) . . ? N2 C6 C7 123.4(2) . . ? C6 C7 C8 118.4(2) . . ? C7 C8 C9 119.7(2) . . ? C8 C9 C10 119.0(2) . . ? N2 C10 C9 121.78(19) . . ? N2 C10 N5 118.48(17) . . ? C9 C10 N5 119.74(19) . . ? N7 C11 C12 123.94(19) . . ? N7 C11 N4 117.95(17) . . ? C12 C11 N4 118.11(18) . . ? C13 C12 C11 117.7(2) . . ? C12 C13 C14 120.00(13) . . ? C13 C14 C15 118.26(13) . . ? N7 C15 C14 123.1(2) . . ? N1 C16 C17 123.85(18) . . ? C16 C17 C18 118.17(18) . . ? C19 C18 C17 119.57(18) . . ? C18 C19 C20 119.28(18) . . ? N1 C20 N3 118.47(15) . . ? N1 C20 C19 121.82(17) . . ? N3 C20 C19 119.71(16) . . ? N8 C21 C22 124.12(19) . . ? N8 C21 N5 115.78(17) . . ? C22 C21 N5 120.10(19) . . ? C21 C22 C23 117.6(2) . . ? C24 C23 C22 118.8(2) . . ? C23 C24 C25 119.0(2) . . ? N8 C25 C24 123.6(2) . . ? C27 C26 N9 124.01(17) . . ? C27 C26 N4 119.12(17) . . ? N9 C26 N4 116.83(17) . . ? C26 C27 C28 117.49(19) . . ? C27 C28 C29 121.5(2) . . ? C28 C29 C30 118.55(19) . . ? N9 C30 C29 121.2(2) . . ? C36 C31 C32 119.65(16) . . ? C33 C32 C31 119.16(16) . . ? C33 C32 N4 119.46(16) . . ? C31 C32 N4 121.27(16) . . ? C34 C33 C32 120.27(17) . . ? C33 C34 C35 120.99(16) . . ? C33 C34 N3 119.63(16) . . ? C35 C34 N3 119.38(15) . . ? C34 C35 C36 118.07(16) . . ? C34 C35 Cu1 89.12(11) . . ? C36 C35 Cu1 92.35(11) . . ? C31 C36 C35 121.31(16) . . ? C31 C36 N5 120.14(16) . . ? C35 C36 N5 118.54(16) . . ? C38 C37 C42 119.4(2) . . ? C38 C37 P1 117.78(16) . . ? C42 C37 P1 122.80(18) . . ? C37 C38 C39 120.5(2) . . ? C40 C39 C38 119.7(3) . . ? C39 C40 C41 120.5(2) . . ? C40 C41 C42 120.7(2) . . ? C37 C42 C41 119.2(3) . . ? C48 C43 C44 118.53(19) . . ? C48 C43 P1 123.14(16) . . ? C44 C43 P1 118.24(16) . . ? C45 C44 C43 120.8(2) . . ? C46 C45 C44 119.5(2) . . ? C47 C46 C45 120.3(2) . . ? C46 C47 C48 120.1(2) . . ? C43 C48 C47 120.6(2) . . ? C54 C49 C50 119.0(2) . . ? C54 C49 P1 124.64(17) . . ? C50 C49 P1 116.31(15) . . ? C51 C50 C49 121.0(2) . . ? C50 C51 C52 119.8(2) . . ? C53 C52 C51 119.7(2) . . ? C52 C53 C54 121.2(2) . . ? C53 C54 C49 119.3(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.556 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.059 # Attachment '4.cif' data_jli2c _database_code_depnum_ccdc_archive 'CCDC 699119' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C109 H87 B2 Cl8 Cu2 F8 N12 P4' _chemical_formula_weight 2273.09 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.823(4) _cell_length_b 17.746(5) _cell_length_c 21.116(5) _cell_angle_alpha 83.863(5) _cell_angle_beta 81.498(6) _cell_angle_gamma 77.153(5) _cell_volume 5340(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2322 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7599 _exptl_absorpt_correction_T_max 0.8684 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24845 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16884 _reflns_number_gt 10895 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0920P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16884 _refine_ls_number_parameters 1215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 0.24806(3) 0.24858(3) -0.03228(2) 0.03178(14) Uani 1 1 d . . . Cu2 Cu 0.26208(3) 0.43127(3) 0.34426(2) 0.03048(14) Uani 1 1 d . . . P1 P 0.32175(7) 0.26557(6) -0.13340(5) 0.0340(3) Uani 1 1 d . . . P2 P 0.21779(7) 0.13118(6) 0.00575(5) 0.0353(3) Uani 1 1 d . . . P3 P 0.14014(7) 0.52707(6) 0.32316(5) 0.0332(3) Uani 1 1 d . . . P4 P 0.36336(7) 0.45935(6) 0.40475(5) 0.0314(3) Uani 1 1 d . . . N1 N 0.2392(2) 0.32087(18) 0.37968(14) 0.0304(8) Uani 1 1 d . . . N2 N 0.3406(2) 0.38376(19) 0.26226(14) 0.0320(8) Uani 1 1 d . . . N3 N 0.2383(2) 0.29718(19) 0.27342(14) 0.0301(8) Uani 1 1 d . . . N4 N 0.1815(2) 0.31839(19) 0.17572(14) 0.0313(8) Uani 1 1 d . . . N5 N 0.1038(2) 0.25334(18) 0.26463(14) 0.0301(8) Uani 1 1 d . . . N6 N 0.0496(2) 0.26896(18) 0.16109(14) 0.0299(8) Uani 1 1 d . . . N7 N -0.1223(2) 0.2171(2) 0.34879(17) 0.0433(9) Uiso 1 1 d . . . N8 N -0.0292(2) 0.21257(19) 0.25075(14) 0.0341(8) Uani 1 1 d . . . N9 N -0.1520(2) 0.2765(2) 0.19146(17) 0.0442(9) Uiso 1 1 d . . . N10 N 0.1058(2) 0.31522(18) -0.02505(14) 0.0323(8) Uani 1 1 d . . . N11 N 0.1298(2) 0.33456(18) 0.07790(14) 0.0293(7) Uani 1 1 d . . . N12 N 0.2812(2) 0.32854(19) 0.02322(14) 0.0320(8) Uani 1 1 d . . . C1 C 0.0441(2) 0.2462(2) 0.22404(18) 0.0308(9) Uani 1 1 d . . . C2 C 0.1710(2) 0.2881(2) 0.23617(18) 0.0305(9) Uani 1 1 d . . . C3 C 0.1178(2) 0.3057(2) 0.14080(17) 0.0282(9) Uani 1 1 d . . . C4 C 0.2418(3) 0.2950(3) 0.4423(2) 0.0440(11) Uani 1 1 d . . . H4B H 0.2468 0.3294 0.4712 0.053 Uiso 1 1 calc R . . C5 C 0.2372(3) 0.2210(3) 0.4649(2) 0.0504(12) Uani 1 1 d . . . H5B H 0.2364 0.2059 0.5085 0.060 Uiso 1 1 calc R . . C6 C 0.2337(3) 0.1686(3) 0.4217(2) 0.0471(11) Uani 1 1 d . . . H6B H 0.2317 0.1175 0.4358 0.056 Uiso 1 1 calc R . . C7 C 0.2333(3) 0.1929(3) 0.3582(2) 0.0424(11) Uani 1 1 d . . . H7B H 0.2312 0.1587 0.3283 0.051 Uiso 1 1 calc R . . C8 C 0.2362(2) 0.2698(2) 0.33900(18) 0.0317(9) Uani 1 1 d . . . C9 C 0.4179(3) 0.4066(3) 0.23277(19) 0.0405(11) Uani 1 1 d . . . H9B H 0.4338 0.4487 0.2477 0.049 Uiso 1 1 calc R . . C10 C 0.4749(3) 0.3716(3) 0.1820(2) 0.0478(12) Uani 1 1 d . . . H10A H 0.5263 0.3909 0.1620 0.057 Uiso 1 1 calc R . . C11 C 0.4538(3) 0.3077(3) 0.1616(2) 0.0506(13) Uani 1 1 d . . . H11A H 0.4914 0.2817 0.1280 0.061 Uiso 1 1 calc R . . C12 C 0.3754(3) 0.2826(3) 0.1919(2) 0.0454(12) Uani 1 1 d . . . H12A H 0.3598 0.2391 0.1791 0.054 Uiso 1 1 calc R . . C13 C 0.3206(2) 0.3219(2) 0.24094(18) 0.0323(10) Uani 1 1 d . . . C14 C -0.1036(3) 0.2097(3) 0.21466(18) 0.0347(10) Uani 1 1 d . . . C15 C -0.1212(3) 0.1385(3) 0.2088(2) 0.0541(13) Uani 1 1 d . . . H15A H -0.0840 0.0933 0.2251 0.065 Uiso 1 1 calc R . . C16 C -0.1967(4) 0.1363(3) 0.1777(3) 0.0712(16) Uani 1 1 d . . . H16A H -0.2113 0.0890 0.1731 0.085 Uiso 1 1 calc R . . C17 C -0.2496(3) 0.2039(4) 0.1539(3) 0.0629(15) Uani 1 1 d . . . H17A H -0.3016 0.2037 0.1342 0.075 Uiso 1 1 calc R . . C18 C -0.2233(3) 0.2721(3) 0.1601(2) 0.0542(13) Uani 1 1 d . . . H18A H -0.2566 0.3177 0.1415 0.065 Uiso 1 1 calc R . . C19 C -0.0409(3) 0.1850(2) 0.31747(18) 0.0329(9) Uani 1 1 d . . . C20 C -0.1393(3) 0.1928(3) 0.4105(2) 0.0502(12) Uani 1 1 d . . . H20A H -0.1964 0.2142 0.4330 0.060 Uiso 1 1 calc R . . C21 C -0.0784(3) 0.1387(3) 0.4427(2) 0.0556(13) Uani 1 1 d . . . H21A H -0.0934 0.1236 0.4858 0.067 Uiso 1 1 calc R . . C22 C 0.0062(3) 0.1071(3) 0.4090(2) 0.0563(13) Uani 1 1 d . . . H22A H 0.0500 0.0702 0.4292 0.068 Uiso 1 1 calc R . . C23 C 0.0250(3) 0.1308(3) 0.3449(2) 0.0433(11) Uani 1 1 d . . . H23A H 0.0813 0.1101 0.3210 0.052 Uiso 1 1 calc R . . C24 C 0.3563(3) 0.3609(3) 0.00736(19) 0.0419(11) Uani 1 1 d . . . H24A H 0.4094 0.3322 -0.0149 0.050 Uiso 1 1 calc R . . C25 C 0.3591(3) 0.4340(3) 0.02213(19) 0.0416(11) Uani 1 1 d . . . H25A H 0.4131 0.4534 0.0106 0.050 Uiso 1 1 calc R . . C26 C 0.2804(3) 0.4777(3) 0.0543(2) 0.0426(11) Uani 1 1 d . . . H26A H 0.2793 0.5279 0.0639 0.051 Uiso 1 1 calc R . . C27 C 0.2029(3) 0.4446(2) 0.07187(19) 0.0394(11) Uani 1 1 d . . . H27A H 0.1485 0.4724 0.0936 0.047 Uiso 1 1 calc R . . C28 C 0.2075(2) 0.3706(2) 0.05676(16) 0.0288(9) Uani 1 1 d . . . C29 C 0.0484(3) 0.3188(2) -0.07060(19) 0.0381(10) Uani 1 1 d . . . H29A H 0.0747 0.3063 -0.1119 0.046 Uiso 1 1 calc R . . C30 C -0.0463(3) 0.3400(3) -0.0577(2) 0.0434(11) Uani 1 1 d . . . H30A H -0.0833 0.3420 -0.0900 0.052 Uiso 1 1 calc R . . C31 C -0.0871(3) 0.3584(3) 0.0036(2) 0.0428(11) Uani 1 1 d . . . H31A H -0.1517 0.3715 0.0132 0.051 Uiso 1 1 calc R . . C32 C -0.0305(3) 0.3569(2) 0.04969(19) 0.0375(10) Uani 1 1 d . . . H32A H -0.0555 0.3701 0.0910 0.045 Uiso 1 1 calc R . . C33 C 0.0655(2) 0.3351(2) 0.03293(17) 0.0280(9) Uani 1 1 d . . . C34 C 0.2602(3) 0.2393(3) -0.19396(19) 0.0433(11) Uani 1 1 d . . . C35 C 0.2105(3) 0.2943(3) -0.2346(2) 0.0563(13) Uani 1 1 d . . . H35A H 0.2087 0.3466 -0.2318 0.068 Uiso 1 1 calc R . . C36 C 0.1636(4) 0.2726(4) -0.2792(3) 0.0742(17) Uani 1 1 d . . . H36A H 0.1300 0.3101 -0.3059 0.089 Uiso 1 1 calc R . . C37 C 0.1667(5) 0.1958(5) -0.2841(3) 0.091(2) Uani 1 1 d . . . H37A H 0.1363 0.1813 -0.3148 0.110 Uiso 1 1 calc R . . C38 C 0.2149(5) 0.1395(4) -0.2436(3) 0.0842(19) Uani 1 1 d . . . H38A H 0.2164 0.0874 -0.2468 0.101 Uiso 1 1 calc R . . C39 C 0.2609(4) 0.1616(3) -0.1982(2) 0.0610(14) Uani 1 1 d . . . H39A H 0.2925 0.1241 -0.1705 0.073 Uiso 1 1 calc R . . C40 C 0.3277(3) 0.3660(2) -0.15900(18) 0.0339(10) Uani 1 1 d . . . C41 C 0.3901(3) 0.3846(3) -0.2116(2) 0.0441(11) Uani 1 1 d . . . H41A H 0.4309 0.3454 -0.2336 0.053 Uiso 1 1 calc R . . C42 C 0.3910(3) 0.4614(3) -0.2308(2) 0.0497(12) Uani 1 1 d . . . H42A H 0.4326 0.4734 -0.2659 0.060 Uiso 1 1 calc R . . C43 C 0.3314(3) 0.5202(3) -0.1991(2) 0.0467(11) Uani 1 1 d . . . H43A H 0.3322 0.5717 -0.2124 0.056 Uiso 1 1 calc R . . C44 C 0.2708(3) 0.5014(3) -0.1471(2) 0.0473(12) Uani 1 1 d . . . H44A H 0.2305 0.5408 -0.1250 0.057 Uiso 1 1 calc R . . C45 C 0.2685(3) 0.4256(2) -0.12739(19) 0.0392(10) Uani 1 1 d . . . H45A H 0.2265 0.4143 -0.0923 0.047 Uiso 1 1 calc R . . C46 C 0.4428(3) 0.2141(2) -0.1535(2) 0.0411(11) Uani 1 1 d . . . C47 C 0.5029(3) 0.2086(3) -0.1087(2) 0.0527(13) Uani 1 1 d . . . H47A H 0.4803 0.2281 -0.0689 0.063 Uiso 1 1 calc R . . C48 C 0.5960(4) 0.1746(3) -0.1218(3) 0.0734(17) Uani 1 1 d . . . H48A H 0.6360 0.1726 -0.0913 0.088 Uiso 1 1 calc R . . C49 C 0.6299(4) 0.1438(3) -0.1795(3) 0.0745(18) Uani 1 1 d . . . H49A H 0.6929 0.1212 -0.1884 0.089 Uiso 1 1 calc R . . C50 C 0.5707(4) 0.1464(3) -0.2240(3) 0.0681(16) Uani 1 1 d . . . H50A H 0.5930 0.1234 -0.2624 0.082 Uiso 1 1 calc R . . C51 C 0.4771(3) 0.1833(3) -0.2121(2) 0.0518(12) Uani 1 1 d . . . H51A H 0.4378 0.1872 -0.2433 0.062 Uiso 1 1 calc R . . C52 C 0.2979(3) 0.0454(3) -0.02534(19) 0.0420(11) Uani 1 1 d . . . C53 C 0.2730(4) -0.0270(3) -0.0194(2) 0.0591(14) Uani 1 1 d . . . H53A H 0.2127 -0.0311 -0.0022 0.071 Uiso 1 1 calc R . . C54 C 0.3368(5) -0.0919(3) -0.0386(3) 0.0729(17) Uani 1 1 d . . . H54A H 0.3197 -0.1398 -0.0347 0.087 Uiso 1 1 calc R . . C55 C 0.4250(4) -0.0855(3) -0.0635(3) 0.0755(18) Uani 1 1 d . . . H55A H 0.4684 -0.1295 -0.0761 0.091 Uiso 1 1 calc R . . C56 C 0.4515(4) -0.0139(3) -0.0703(3) 0.0725(17) Uani 1 1 d . . . H56A H 0.5119 -0.0101 -0.0876 0.087 Uiso 1 1 calc R . . C57 C 0.3877(3) 0.0502(3) -0.0512(2) 0.0495(12) Uani 1 1 d . . . H57A H 0.4049 0.0979 -0.0556 0.059 Uiso 1 1 calc R . . C58 C 0.1045(3) 0.1237(2) -0.0136(2) 0.0419(11) Uani 1 1 d . . . C59 C 0.0225(3) 0.1542(3) 0.0255(2) 0.0497(12) Uani 1 1 d . . . H59A H 0.0261 0.1740 0.0639 0.060 Uiso 1 1 calc R . . C60 C -0.0637(4) 0.1553(3) 0.0075(3) 0.0642(15) Uani 1 1 d . . . H60A H -0.1178 0.1741 0.0345 0.077 Uiso 1 1 calc R . . C61 C -0.0695(4) 0.1289(4) -0.0495(3) 0.0787(19) Uani 1 1 d . . . H61A H -0.1279 0.1310 -0.0617 0.094 Uiso 1 1 calc R . . C62 C 0.0082(4) 0.0997(4) -0.0887(3) 0.0789(18) Uani 1 1 d . . . H62A H 0.0029 0.0815 -0.1274 0.095 Uiso 1 1 calc R . . C63 C 0.0968(4) 0.0967(3) -0.0715(2) 0.0604(14) Uani 1 1 d . . . H63A H 0.1501 0.0768 -0.0987 0.073 Uiso 1 1 calc R . . C64 C 0.2160(3) 0.1031(2) 0.09200(19) 0.0383(11) Uani 1 1 d . . . C65 C 0.2813(4) 0.1241(3) 0.1225(2) 0.0529(13) Uani 1 1 d . . . H65A H 0.3176 0.1576 0.1008 0.064 Uiso 1 1 calc R . . C66 C 0.2940(4) 0.0961(3) 0.1854(2) 0.0664(16) Uani 1 1 d . . . H66A H 0.3404 0.1087 0.2049 0.080 Uiso 1 1 calc R . . C67 C 0.2365(5) 0.0492(3) 0.2186(2) 0.0688(18) Uani 1 1 d . . . H67A H 0.2433 0.0308 0.2610 0.083 Uiso 1 1 calc R . . C68 C 0.1712(4) 0.0304(3) 0.1894(2) 0.0668(16) Uani 1 1 d . . . H68A H 0.1321 -0.0003 0.2122 0.080 Uiso 1 1 calc R . . C69 C 0.1602(3) 0.0556(3) 0.1261(2) 0.0526(13) Uani 1 1 d . . . H69A H 0.1155 0.0405 0.1065 0.063 Uiso 1 1 calc R . . C70 C 0.0457(3) 0.4932(3) 0.2967(2) 0.0435(11) Uani 1 1 d . . . C71 C 0.0010(4) 0.5271(3) 0.2445(3) 0.0708(17) Uani 1 1 d . . . H71A H 0.0176 0.5707 0.2215 0.085 Uiso 1 1 calc R . . C72 C -0.0683(4) 0.4962(4) 0.2262(4) 0.097(2) Uani 1 1 d . . . H72A H -0.0980 0.5198 0.1912 0.116 Uiso 1 1 calc R . . C73 C -0.0939(4) 0.4329(4) 0.2579(4) 0.090(2) Uani 1 1 d . . . H73A H -0.1402 0.4130 0.2443 0.108 Uiso 1 1 calc R . . C74 C -0.0519(3) 0.3974(3) 0.3104(3) 0.0730(18) Uani 1 1 d . . . H74A H -0.0697 0.3539 0.3328 0.088 Uiso 1 1 calc R . . C75 C 0.0194(3) 0.4284(3) 0.3298(3) 0.0545(13) Uani 1 1 d . . . H75A H 0.0486 0.4048 0.3651 0.065 Uiso 1 1 calc R . . C76 C 0.1638(3) 0.6027(2) 0.26102(19) 0.0370(10) Uani 1 1 d . . . C77 C 0.2379(3) 0.5846(3) 0.21294(19) 0.0423(11) Uani 1 1 d . . . H77A H 0.2733 0.5343 0.2124 0.051 Uiso 1 1 calc R . . C78 C 0.2598(4) 0.6409(3) 0.1655(2) 0.0571(13) Uani 1 1 d . . . H78A H 0.3106 0.6290 0.1340 0.069 Uiso 1 1 calc R . . C79 C 0.2043(5) 0.7151(3) 0.1662(2) 0.0698(16) Uani 1 1 d . . . H79A H 0.2182 0.7532 0.1348 0.084 Uiso 1 1 calc R . . C80 C 0.1303(5) 0.7327(3) 0.2119(3) 0.0754(18) Uani 1 1 d . . . H80A H 0.0932 0.7824 0.2111 0.090 Uiso 1 1 calc R . . C81 C 0.1093(4) 0.6775(3) 0.2599(2) 0.0572(14) Uani 1 1 d . . . H81A H 0.0587 0.6903 0.2914 0.069 Uiso 1 1 calc R . . C82 C 0.0870(3) 0.5844(2) 0.3918(2) 0.0370(10) Uani 1 1 d . . . C83 C 0.0091(4) 0.5717(4) 0.4307(3) 0.100(2) Uani 1 1 d . . . H83A H -0.0227 0.5354 0.4213 0.120 Uiso 1 1 calc R . . C84 C -0.0230(5) 0.6138(5) 0.4853(4) 0.130(3) Uani 1 1 d . . . H84A H -0.0747 0.6034 0.5127 0.157 Uiso 1 1 calc R . . C85 C 0.0192(5) 0.6686(4) 0.4991(3) 0.084(2) Uani 1 1 d . . . H85A H -0.0054 0.6984 0.5336 0.101 Uiso 1 1 calc R . . C86 C 0.0972(4) 0.6792(3) 0.4622(2) 0.0587(14) Uani 1 1 d . . . H86A H 0.1288 0.7152 0.4724 0.070 Uiso 1 1 calc R . . C87 C 0.1314(3) 0.6378(3) 0.4092(2) 0.0475(12) Uani 1 1 d . . . H87A H 0.1862 0.6461 0.3845 0.057 Uiso 1 1 calc R . . C88 C 0.4828(3) 0.4037(2) 0.38544(18) 0.0336(10) Uani 1 1 d . . . C89 C 0.4931(3) 0.3287(3) 0.3685(2) 0.0510(12) Uani 1 1 d . . . H89A H 0.4407 0.3077 0.3695 0.061 Uiso 1 1 calc R . . C90 C 0.5808(3) 0.2849(3) 0.3500(2) 0.0600(14) Uani 1 1 d . . . H90A H 0.5874 0.2346 0.3385 0.072 Uiso 1 1 calc R . . C91 C 0.6591(3) 0.3163(3) 0.3487(2) 0.0599(15) Uani 1 1 d . . . H91A H 0.7184 0.2876 0.3360 0.072 Uiso 1 1 calc R . . C92 C 0.6476(3) 0.3891(3) 0.3662(2) 0.0541(13) Uani 1 1 d . . . H92A H 0.6999 0.4102 0.3653 0.065 Uiso 1 1 calc R . . C93 C 0.5605(3) 0.4334(3) 0.3852(2) 0.0438(11) Uani 1 1 d . . . H93A H 0.5548 0.4830 0.3979 0.053 Uiso 1 1 calc R . . C94 C 0.3736(2) 0.5608(2) 0.39436(19) 0.0331(9) Uani 1 1 d . . . C95 C 0.3661(3) 0.6852(3) 0.4322(2) 0.0534(13) Uani 1 1 d . . . H95A H 0.3613 0.7154 0.4664 0.064 Uiso 1 1 calc R . . C96 C 0.3755(3) 0.5960(2) 0.3318(2) 0.0391(10) Uani 1 1 d . . . H96A H 0.3774 0.5666 0.2975 0.047 Uiso 1 1 calc R . . C97 C 0.3745(3) 0.6745(3) 0.3208(2) 0.0479(12) Uani 1 1 d . . . H97A H 0.3773 0.6972 0.2789 0.058 Uiso 1 1 calc R . . C98 C 0.3695(3) 0.7194(3) 0.3712(3) 0.0547(13) Uani 1 1 d . . . H98A H 0.3685 0.7722 0.3637 0.066 Uiso 1 1 calc R . . C99 C 0.3697(3) 0.6063(3) 0.4445(2) 0.0429(11) Uani 1 1 d . . . H99A H 0.3695 0.5840 0.4864 0.051 Uiso 1 1 calc R . . C100 C 0.3363(3) 0.4421(2) 0.49132(18) 0.0351(10) Uani 1 1 d . . . C101 C 0.2486(3) 0.4772(3) 0.5210(2) 0.0502(12) Uani 1 1 d . . . H10B H 0.2054 0.5084 0.4965 0.060 Uiso 1 1 calc R . . C102 C 0.2261(3) 0.4658(3) 0.5858(2) 0.0605(14) Uani 1 1 d . . . H10C H 0.1681 0.4904 0.6052 0.073 Uiso 1 1 calc R . . C103 C 0.2879(4) 0.4183(3) 0.6230(2) 0.0631(15) Uani 1 1 d . . . H10D H 0.2718 0.4108 0.6672 0.076 Uiso 1 1 calc R . . C104 C 0.3724(4) 0.3827(3) 0.5947(2) 0.0590(14) Uani 1 1 d . . . H10E H 0.4141 0.3501 0.6197 0.071 Uiso 1 1 calc R . . C105 C 0.3978(3) 0.3941(3) 0.5292(2) 0.0418(11) Uani 1 1 d . . . H10F H 0.4562 0.3694 0.5105 0.050 Uiso 1 1 calc R . . F1 F 0.5801(2) 0.27422(16) 0.02905(15) 0.0760(10) Uani 1 1 d . . . F2 F 0.58896(19) 0.38191(17) -0.03489(13) 0.0701(9) Uani 1 1 d . . . F3 F 0.72085(17) 0.29489(19) -0.01587(13) 0.0757(9) Uani 1 1 d . . . F4 F 0.6371(2) 0.3680(2) 0.06214(15) 0.0870(10) Uani 1 1 d . . . F5 F 0.2848(8) -0.1237(6) 0.4424(5) 0.115(4) Uani 0.60 1 d P . . F6 F 0.1907(5) -0.0171(4) 0.4323(4) 0.111(3) Uani 0.60 1 d P . . F7 F 0.3379(5) -0.0596(6) 0.3654(3) 0.128(3) Uani 0.60 1 d P . . F7A F 0.3210(14) -0.0159(8) 0.4083(17) 0.311(17) Uani 0.40 1 d P . . F6A F 0.2085(11) 0.0031(6) 0.3813(7) 0.131(5) Uani 0.40 1 d P . . F8 F 0.2323(5) -0.0935(4) 0.3449(3) 0.188(2) Uani 1 1 d . . . F5A F 0.2373(18) -0.1193(14) 0.4345(9) 0.212(13) Uani 0.40 1 d P . . B1 B 0.6332(3) 0.3303(3) 0.0101(2) 0.0448(13) Uani 1 1 d . . . B2 B 0.2574(7) -0.0628(5) 0.3988(4) 0.087(2) 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 0.0329(3) 0.0324(3) 0.0305(3) -0.0040(2) -0.0039(2) -0.0072(2) Cu2 0.0264(2) 0.0355(3) 0.0297(3) -0.0066(2) -0.00453(19) -0.0041(2) P1 0.0362(6) 0.0370(6) 0.0298(6) -0.0049(5) -0.0033(4) -0.0094(5) P2 0.0389(6) 0.0319(6) 0.0361(6) -0.0033(5) -0.0052(5) -0.0091(5) P3 0.0250(5) 0.0386(6) 0.0358(6) -0.0074(5) -0.0064(4) -0.0022(5) P4 0.0248(5) 0.0363(6) 0.0336(6) -0.0055(4) -0.0071(4) -0.0037(5) N1 0.0292(16) 0.038(2) 0.0236(17) -0.0031(14) -0.0047(13) -0.0062(15) N2 0.0263(16) 0.040(2) 0.0300(18) -0.0074(15) 0.0005(13) -0.0074(16) N3 0.0284(16) 0.039(2) 0.0262(17) -0.0060(14) -0.0040(13) -0.0111(15) N4 0.0265(16) 0.042(2) 0.0284(18) -0.0052(15) -0.0048(13) -0.0113(15) N5 0.0276(16) 0.033(2) 0.0299(18) -0.0053(14) -0.0026(14) -0.0068(15) N6 0.0275(16) 0.035(2) 0.0289(18) -0.0034(14) -0.0046(13) -0.0089(15) N8 0.0326(17) 0.044(2) 0.0284(18) -0.0012(15) -0.0035(14) -0.0141(16) N10 0.0392(18) 0.0318(19) 0.0284(18) -0.0026(14) -0.0099(14) -0.0089(16) N11 0.0294(16) 0.038(2) 0.0251(17) -0.0025(14) -0.0078(13) -0.0138(15) N12 0.0292(17) 0.042(2) 0.0279(18) -0.0038(15) -0.0067(14) -0.0103(16) C1 0.0255(19) 0.031(2) 0.036(2) -0.0068(17) -0.0067(16) -0.0027(18) C2 0.0263(19) 0.033(2) 0.032(2) -0.0086(17) -0.0058(16) -0.0030(18) C3 0.028(2) 0.024(2) 0.032(2) -0.0075(16) -0.0062(16) 0.0011(18) C4 0.052(3) 0.048(3) 0.037(3) -0.009(2) -0.007(2) -0.016(2) C5 0.064(3) 0.056(3) 0.036(3) 0.001(2) -0.016(2) -0.019(3) C6 0.052(3) 0.038(3) 0.054(3) 0.005(2) -0.015(2) -0.013(2) C7 0.045(2) 0.042(3) 0.042(3) -0.012(2) -0.011(2) -0.004(2) C8 0.0268(19) 0.034(2) 0.032(2) -0.0034(18) -0.0056(16) -0.0011(18) C9 0.034(2) 0.052(3) 0.040(2) -0.008(2) -0.0043(19) -0.015(2) C10 0.027(2) 0.077(4) 0.039(3) -0.010(2) 0.0005(18) -0.012(2) C11 0.034(2) 0.079(4) 0.040(3) -0.026(2) 0.0057(19) -0.011(2) C12 0.037(2) 0.063(3) 0.042(3) -0.025(2) -0.0004(19) -0.016(2) C13 0.0225(19) 0.042(3) 0.032(2) -0.0067(19) -0.0072(16) -0.0033(19) C14 0.028(2) 0.045(3) 0.033(2) -0.0059(19) -0.0009(16) -0.012(2) C15 0.063(3) 0.044(3) 0.064(3) 0.007(2) -0.024(3) -0.022(3) C16 0.085(4) 0.061(4) 0.090(4) 0.002(3) -0.039(3) -0.046(3) C17 0.045(3) 0.083(4) 0.073(4) -0.008(3) -0.022(2) -0.029(3) C18 0.038(2) 0.063(4) 0.063(3) -0.003(3) -0.015(2) -0.009(3) C19 0.033(2) 0.034(2) 0.035(2) -0.0062(18) -0.0016(17) -0.0152(19) C20 0.048(3) 0.062(3) 0.036(3) -0.005(2) 0.007(2) -0.010(2) C21 0.064(3) 0.068(4) 0.037(3) -0.001(2) -0.002(2) -0.025(3) C22 0.057(3) 0.054(3) 0.056(3) 0.007(2) -0.014(2) -0.008(3) C23 0.037(2) 0.044(3) 0.046(3) 0.000(2) 0.0000(19) -0.007(2) C24 0.032(2) 0.057(3) 0.038(2) -0.009(2) -0.0045(18) -0.010(2) C25 0.038(2) 0.055(3) 0.038(2) -0.002(2) -0.0040(19) -0.023(2) C26 0.050(3) 0.036(3) 0.047(3) -0.008(2) -0.009(2) -0.017(2) C27 0.043(2) 0.039(3) 0.038(2) -0.0101(19) -0.0050(19) -0.009(2) C28 0.030(2) 0.037(2) 0.0212(19) -0.0001(16) -0.0118(16) -0.0064(18) C29 0.044(2) 0.040(3) 0.033(2) -0.0012(18) -0.0131(18) -0.011(2) C30 0.035(2) 0.052(3) 0.047(3) 0.003(2) -0.021(2) -0.009(2) C31 0.028(2) 0.052(3) 0.051(3) 0.004(2) -0.0174(19) -0.009(2) C32 0.030(2) 0.043(3) 0.036(2) -0.0055(19) -0.0054(17) -0.0007(19) C33 0.0298(19) 0.027(2) 0.031(2) 0.0017(16) -0.0106(16) -0.0103(17) C34 0.048(3) 0.058(3) 0.031(2) -0.011(2) -0.0020(19) -0.023(2) C35 0.058(3) 0.071(4) 0.045(3) -0.008(3) -0.013(2) -0.020(3) C36 0.073(4) 0.103(5) 0.059(4) -0.003(3) -0.025(3) -0.034(4) C37 0.108(5) 0.131(7) 0.065(4) -0.008(4) -0.032(4) -0.076(5) C38 0.113(5) 0.089(5) 0.073(4) -0.012(4) -0.015(4) -0.066(4) C39 0.084(4) 0.065(4) 0.047(3) -0.007(3) -0.014(3) -0.038(3) C40 0.033(2) 0.038(2) 0.034(2) -0.0037(18) -0.0108(17) -0.0104(19) C41 0.039(2) 0.047(3) 0.044(3) -0.003(2) 0.0024(19) -0.010(2) C42 0.046(3) 0.054(3) 0.049(3) 0.007(2) 0.000(2) -0.018(2) C43 0.048(3) 0.041(3) 0.055(3) 0.008(2) -0.017(2) -0.016(2) C44 0.043(3) 0.039(3) 0.059(3) -0.003(2) -0.010(2) -0.004(2) C45 0.038(2) 0.044(3) 0.034(2) -0.0039(19) -0.0035(18) -0.007(2) C46 0.041(2) 0.035(3) 0.044(3) -0.006(2) 0.003(2) -0.005(2) C47 0.043(3) 0.054(3) 0.060(3) -0.011(2) -0.006(2) -0.004(2) C48 0.053(3) 0.073(4) 0.090(4) -0.009(3) -0.017(3) 0.005(3) C49 0.041(3) 0.056(4) 0.119(5) -0.008(4) 0.009(3) -0.006(3) C50 0.073(4) 0.045(3) 0.077(4) -0.014(3) 0.026(3) -0.012(3) C51 0.051(3) 0.047(3) 0.054(3) -0.012(2) 0.006(2) -0.007(2) C52 0.056(3) 0.037(3) 0.034(2) -0.0064(19) -0.006(2) -0.008(2) C53 0.079(4) 0.040(3) 0.059(3) -0.010(2) 0.004(3) -0.018(3) C54 0.111(5) 0.035(3) 0.070(4) -0.016(3) -0.006(3) -0.008(3) C55 0.085(4) 0.049(4) 0.081(4) -0.022(3) -0.002(3) 0.012(3) C56 0.064(3) 0.060(4) 0.088(4) -0.022(3) 0.001(3) 0.000(3) C57 0.048(3) 0.042(3) 0.056(3) -0.009(2) -0.003(2) -0.006(2) C58 0.047(3) 0.033(3) 0.049(3) 0.005(2) -0.011(2) -0.016(2) C59 0.047(3) 0.039(3) 0.063(3) 0.005(2) -0.010(2) -0.010(2) C60 0.047(3) 0.065(4) 0.080(4) 0.018(3) -0.010(3) -0.019(3) C61 0.059(4) 0.089(5) 0.098(5) 0.042(4) -0.033(4) -0.043(3) C62 0.075(4) 0.110(5) 0.069(4) 0.007(3) -0.031(3) -0.046(4) C63 0.065(3) 0.074(4) 0.049(3) 0.002(3) -0.014(2) -0.027(3) C64 0.041(2) 0.031(2) 0.037(2) -0.0075(19) -0.0017(19) 0.004(2) C65 0.069(3) 0.042(3) 0.044(3) -0.006(2) -0.009(2) -0.002(3) C66 0.096(4) 0.054(3) 0.047(3) -0.013(3) -0.027(3) 0.006(3) C67 0.104(5) 0.048(3) 0.037(3) -0.007(2) -0.002(3) 0.017(3) C68 0.082(4) 0.059(4) 0.043(3) 0.009(3) 0.014(3) 0.000(3) C69 0.056(3) 0.054(3) 0.043(3) 0.005(2) -0.001(2) -0.008(2) C70 0.025(2) 0.041(3) 0.067(3) -0.016(2) -0.012(2) -0.004(2) C71 0.066(3) 0.052(3) 0.106(5) -0.017(3) -0.053(3) -0.004(3) C72 0.082(4) 0.075(5) 0.153(7) -0.027(5) -0.079(4) -0.011(4) C73 0.042(3) 0.071(5) 0.172(7) -0.063(5) -0.039(4) 0.001(3) C74 0.037(3) 0.042(3) 0.143(6) -0.045(3) 0.010(3) -0.009(3) C75 0.029(2) 0.046(3) 0.088(4) -0.024(3) -0.003(2) 0.000(2) C76 0.041(2) 0.036(2) 0.037(2) -0.0070(18) -0.0140(18) -0.007(2) C77 0.051(3) 0.049(3) 0.030(2) -0.001(2) -0.0110(19) -0.015(2) C78 0.067(3) 0.071(4) 0.039(3) -0.003(2) -0.009(2) -0.026(3) C79 0.117(5) 0.053(3) 0.043(3) 0.003(3) -0.015(3) -0.027(3) C80 0.115(5) 0.048(3) 0.055(3) 0.002(3) -0.013(3) 0.000(3) C81 0.067(3) 0.051(3) 0.045(3) -0.001(2) -0.003(2) 0.000(3) C82 0.033(2) 0.033(2) 0.045(3) -0.0100(19) -0.0004(18) -0.006(2) C83 0.075(4) 0.089(5) 0.137(6) -0.069(4) 0.061(4) -0.041(4) C84 0.113(6) 0.131(7) 0.148(7) -0.090(6) 0.085(5) -0.055(5) C85 0.107(5) 0.065(4) 0.078(4) -0.039(3) 0.031(4) -0.027(4) C86 0.060(3) 0.061(3) 0.055(3) -0.025(3) -0.007(3) -0.002(3) C87 0.029(2) 0.062(3) 0.050(3) -0.017(2) -0.0046(19) 0.000(2) C88 0.028(2) 0.042(3) 0.029(2) -0.0010(18) -0.0060(16) -0.0019(19) C89 0.040(2) 0.044(3) 0.067(3) -0.009(2) -0.014(2) 0.001(2) C90 0.048(3) 0.051(3) 0.075(4) -0.009(3) -0.013(2) 0.008(3) C91 0.041(3) 0.072(4) 0.052(3) 0.009(3) 0.000(2) 0.010(3) C92 0.027(2) 0.072(4) 0.056(3) 0.009(3) -0.002(2) -0.005(2) C93 0.033(2) 0.055(3) 0.042(3) 0.000(2) -0.0026(18) -0.009(2) C94 0.0238(19) 0.037(2) 0.041(2) -0.0066(19) -0.0086(17) -0.0059(18) C95 0.051(3) 0.045(3) 0.065(3) -0.019(3) -0.008(2) -0.005(2) C96 0.038(2) 0.039(3) 0.040(3) -0.0086(19) -0.0079(18) -0.003(2) C97 0.044(3) 0.044(3) 0.052(3) 0.000(2) -0.006(2) -0.004(2) C98 0.048(3) 0.041(3) 0.073(4) -0.007(3) -0.006(2) -0.006(2) C99 0.039(2) 0.046(3) 0.047(3) -0.010(2) -0.0084(19) -0.009(2) C100 0.034(2) 0.039(2) 0.035(2) -0.0090(18) -0.0092(17) -0.0082(19) C101 0.038(2) 0.075(4) 0.038(3) -0.015(2) -0.0074(19) -0.006(2) C102 0.038(3) 0.091(4) 0.053(3) -0.021(3) 0.005(2) -0.014(3) C103 0.065(3) 0.094(4) 0.038(3) 0.005(3) -0.005(2) -0.038(3) C104 0.063(3) 0.070(4) 0.045(3) 0.006(2) -0.013(2) -0.017(3) C105 0.042(2) 0.047(3) 0.039(3) -0.002(2) -0.0088(19) -0.014(2) F1 0.072(2) 0.0484(18) 0.095(2) -0.0044(16) 0.0251(17) -0.0094(16) F2 0.0580(17) 0.085(2) 0.0568(18) 0.0135(15) -0.0087(14) 0.0000(15) F3 0.0385(15) 0.120(3) 0.0560(18) 0.0019(17) 0.0013(13) 0.0014(16) F4 0.096(2) 0.108(3) 0.065(2) -0.0256(19) -0.0196(17) -0.021(2) F5 0.163(9) 0.080(6) 0.089(6) -0.030(5) -0.048(6) 0.035(6) F6 0.104(5) 0.073(5) 0.129(6) -0.027(5) 0.017(5) 0.025(4) F7 0.074(5) 0.217(10) 0.085(5) 0.006(5) 0.018(4) -0.046(6) F7A 0.120(13) 0.058(8) 0.74(6) -0.060(16) 0.00(2) -0.019(9) F6A 0.188(13) 0.057(7) 0.129(10) -0.015(7) -0.058(10) 0.045(7) F8 0.239(7) 0.170(5) 0.154(5) -0.008(4) -0.053(5) -0.025(5) F5A 0.27(3) 0.20(2) 0.127(16) 0.035(13) 0.114(17) -0.080(18) B1 0.038(3) 0.057(4) 0.038(3) -0.004(3) -0.001(2) -0.009(3) B2 0.094(6) 0.071(6) 0.088(6) -0.009(5) -0.018(5) 0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N12 2.113(3) . ? Cu1 N10 2.169(3) . ? Cu1 P2 2.2667(13) . ? Cu1 P1 2.2721(12) . ? Cu2 N2 2.084(3) . ? Cu2 N1 2.102(3) . ? Cu2 P3 2.2507(11) . ? Cu2 P4 2.2736(12) . ? P1 C40 1.824(4) . ? P1 C34 1.830(4) . ? P1 C46 1.834(4) . ? P2 C58 1.822(5) . ? P2 C52 1.827(4) . ? P2 C64 1.834(4) . ? P3 C70 1.819(4) . ? P3 C76 1.828(4) . ? P3 C82 1.837(4) . ? P4 C100 1.820(4) . ? P4 C94 1.828(4) . ? P4 C88 1.836(4) . ? N1 C8 1.326(5) . ? N1 C4 1.355(5) . ? N2 C13 1.336(5) . ? N2 C9 1.344(5) . ? N3 C2 1.403(5) . ? N3 C8 1.416(5) . ? N3 C13 1.442(5) . ? N4 C2 1.332(5) . ? N4 C3 1.349(5) . ? N5 C2 1.323(5) . ? N5 C1 1.353(5) . ? N6 C3 1.317(5) . ? N6 C1 1.344(5) . ? N7 C19 1.325(5) . ? N7 C20 1.333(5) . ? N8 C1 1.375(5) . ? N8 C19 1.440(5) . ? N8 C14 1.443(5) . ? N9 C14 1.327(5) . ? N9 C18 1.348(6) . ? N10 C33 1.328(5) . ? N10 C29 1.363(5) . ? N11 C3 1.372(5) . ? N11 C28 1.431(5) . ? N11 C33 1.439(5) . ? N12 C28 1.332(5) . ? N12 C24 1.347(5) . ? C4 C5 1.362(6) . ? C5 C6 1.383(6) . ? C6 C7 1.364(6) . ? C7 C8 1.389(6) . ? C9 C10 1.375(6) . ? C10 C11 1.368(6) . ? C11 C12 1.381(6) . ? C12 C13 1.368(5) . ? C14 C15 1.366(6) . ? C15 C16 1.389(7) . ? C16 C17 1.371(7) . ? C17 C18 1.375(7) . ? C19 C23 1.358(6) . ? C20 C21 1.361(6) . ? C21 C22 1.379(6) . ? C22 C23 1.381(6) . ? C24 C25 1.376(6) . ? C25 C26 1.379(6) . ? C26 C27 1.390(6) . ? C27 C28 1.370(5) . ? C29 C30 1.363(6) . ? C30 C31 1.386(6) . ? C31 C32 1.372(6) . ? C32 C33 1.391(5) . ? C34 C35 1.386(6) . ? C34 C39 1.388(7) . ? C35 C36 1.382(7) . ? C36 C37 1.368(9) . ? C37 C38 1.385(9) . ? C38 C39 1.390(7) . ? C40 C45 1.378(5) . ? C40 C41 1.397(6) . ? C41 C42 1.383(6) . ? C42 C43 1.372(6) . ? C43 C44 1.373(6) . ? C44 C45 1.372(6) . ? C46 C47 1.373(6) . ? C46 C51 1.386(6) . ? C47 C48 1.378(7) . ? C48 C49 1.371(8) . ? C49 C50 1.367(8) . ? C50 C51 1.395(7) . ? C52 C57 1.379(6) . ? C52 C53 1.402(6) . ? C53 C54 1.374(7) . ? C54 C55 1.359(8) . ? C55 C56 1.399(8) . ? C56 C57 1.364(6) . ? C58 C63 1.388(6) . ? C58 C59 1.398(6) . ? C59 C60 1.382(7) . ? C60 C61 1.357(8) . ? C61 C62 1.352(8) . ? C62 C63 1.403(7) . ? C64 C65 1.373(6) . ? C64 C69 1.385(6) . ? C65 C66 1.392(6) . ? C66 C67 1.388(8) . ? C67 C68 1.340(8) . ? C68 C69 1.385(7) . ? C70 C75 1.382(7) . ? C70 C71 1.384(7) . ? C71 C72 1.385(8) . ? C72 C73 1.344(9) . ? C73 C74 1.376(9) . ? C74 C75 1.421(7) . ? C76 C77 1.387(6) . ? C76 C81 1.392(6) . ? C77 C78 1.393(6) . ? C78 C79 1.389(7) . ? C79 C80 1.354(8) . ? C80 C81 1.383(7) . ? C82 C83 1.363(7) . ? C82 C87 1.375(6) . ? C83 C84 1.406(8) . ? C84 C85 1.344(9) . ? C85 C86 1.333(7) . ? C86 C87 1.375(6) . ? C88 C93 1.369(6) . ? C88 C89 1.385(6) . ? C89 C90 1.382(6) . ? C90 C91 1.391(7) . ? C91 C92 1.349(7) . ? C92 C93 1.381(6) . ? C94 C99 1.386(6) . ? C94 C96 1.398(6) . ? C95 C98 1.362(7) . ? C95 C99 1.386(6) . ? C96 C97 1.384(6) . ? C97 C98 1.382(6) . ? C100 C105 1.386(5) . ? C100 C101 1.397(5) . ? C101 C102 1.364(6) . ? C102 C103 1.376(7) . ? C103 C104 1.354(7) . ? C104 C105 1.385(6) . ? F1 B1 1.392(6) . ? F2 B1 1.379(6) . ? F3 B1 1.373(5) . ? F4 B1 1.361(6) . ? F5 F5A 0.73(3) . ? F5 B2 1.372(13) . ? F6 F6A 1.110(12) . ? F6 B2 1.302(10) . ? F7 F7A 1.22(3) . ? F7 B2 1.303(12) . ? F7A B2 1.44(2) . ? F6A B2 1.280(12) . ? F8 B2 1.441(10) . ? F5A B2 1.25(2) . ? 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 N12 Cu1 N10 88.72(12) . . ? N12 Cu1 P2 125.23(9) . . ? N10 Cu1 P2 98.53(9) . . ? N12 Cu1 P1 107.12(9) . . ? N10 Cu1 P1 110.20(9) . . ? P2 Cu1 P1 120.27(4) . . ? N2 Cu2 N1 89.61(13) . . ? N2 Cu2 P3 113.56(9) . . ? N1 Cu2 P3 119.65(9) . . ? N2 Cu2 P4 107.30(10) . . ? N1 Cu2 P4 106.36(9) . . ? P3 Cu2 P4 116.71(5) . . ? C40 P1 C34 103.0(2) . . ? C40 P1 C46 102.47(19) . . ? C34 P1 C46 103.9(2) . . ? C40 P1 Cu1 114.02(13) . . ? C34 P1 Cu1 112.12(14) . . ? C46 P1 Cu1 119.48(14) . . ? C58 P2 C52 104.3(2) . . ? C58 P2 C64 105.7(2) . . ? C52 P2 C64 99.12(18) . . ? C58 P2 Cu1 109.82(14) . . ? C52 P2 Cu1 117.51(15) . . ? C64 P2 Cu1 118.78(15) . . ? C70 P3 C76 103.6(2) . . ? C70 P3 C82 105.92(19) . . ? C76 P3 C82 101.60(19) . . ? C70 P3 Cu2 113.58(15) . . ? C76 P3 Cu2 116.73(13) . . ? C82 P3 Cu2 113.99(14) . . ? C100 P4 C94 103.40(19) . . ? C100 P4 C88 104.96(17) . . ? C94 P4 C88 104.96(18) . . ? C100 P4 Cu2 116.07(14) . . ? C94 P4 Cu2 113.81(13) . . ? C88 P4 Cu2 112.52(14) . . ? C8 N1 C4 117.3(4) . . ? C8 N1 Cu2 119.7(3) . . ? C4 N1 Cu2 122.2(3) . . ? C13 N2 C9 116.7(3) . . ? C13 N2 Cu2 119.6(2) . . ? C9 N2 Cu2 123.4(3) . . ? C2 N3 C8 122.1(3) . . ? C2 N3 C13 118.2(3) . . ? C8 N3 C13 118.8(3) . . ? C2 N4 C3 113.0(3) . . ? C2 N5 C1 112.7(3) . . ? C3 N6 C1 113.4(3) . . ? C19 N7 C20 116.8(4) . . ? C1 N8 C19 122.2(3) . . ? C1 N8 C14 121.4(3) . . ? C19 N8 C14 116.1(3) . . ? C14 N9 C18 116.2(4) . . ? C33 N10 C29 116.9(3) . . ? C33 N10 Cu1 117.0(2) . . ? C29 N10 Cu1 123.4(3) . . ? C3 N11 C28 118.2(3) . . ? C3 N11 C33 123.7(3) . . ? C28 N11 C33 117.9(3) . . ? C28 N12 C24 116.2(3) . . ? C28 N12 Cu1 114.2(2) . . ? C24 N12 Cu1 123.6(3) . . ? N6 C1 N5 126.4(4) . . ? N6 C1 N8 117.7(3) . . ? N5 C1 N8 115.9(3) . . ? N5 C2 N4 127.5(3) . . ? N5 C2 N3 117.6(3) . . ? N4 C2 N3 114.8(3) . . ? N6 C3 N4 126.7(3) . . ? N6 C3 N11 119.8(3) . . ? N4 C3 N11 113.5(3) . . ? N1 C4 C5 123.1(4) . . ? C4 C5 C6 118.7(4) . . ? C7 C6 C5 119.2(4) . . ? C6 C7 C8 118.8(4) . . ? N1 C8 C7 122.9(4) . . ? N1 C8 N3 116.3(3) . . ? C7 C8 N3 120.8(4) . . ? N2 C9 C10 124.2(4) . . ? C11 C10 C9 118.1(4) . . ? C10 C11 C12 118.6(4) . . ? C13 C12 C11 119.9(4) . . ? N2 C13 C12 122.6(4) . . ? N2 C13 N3 116.3(3) . . ? C12 C13 N3 121.1(4) . . ? N9 C14 C15 124.8(4) . . ? N9 C14 N8 117.6(4) . . ? C15 C14 N8 117.5(4) . . ? C14 C15 C16 117.4(5) . . ? C17 C16 C15 119.8(5) . . ? C16 C17 C18 117.9(5) . . ? N9 C18 C17 123.8(5) . . ? N7 C19 C23 123.8(4) . . ? N7 C19 N8 113.3(3) . . ? C23 C19 N8 122.9(3) . . ? N7 C20 C21 124.3(4) . . ? C20 C21 C22 117.6(4) . . ? C21 C22 C23 119.2(4) . . ? C19 C23 C22 118.4(4) . . ? N12 C24 C25 124.0(4) . . ? C24 C25 C26 118.7(4) . . ? C25 C26 C27 118.0(4) . . ? C28 C27 C26 119.1(4) . . ? N12 C28 C27 123.9(4) . . ? N12 C28 N11 116.7(3) . . ? C27 C28 N11 119.4(3) . . ? C30 C29 N10 122.3(4) . . ? C29 C30 C31 119.9(4) . . ? C32 C31 C30 118.7(4) . . ? C31 C32 C33 118.2(4) . . ? N10 C33 C32 123.9(4) . . ? N10 C33 N11 114.4(3) . . ? C32 C33 N11 121.6(3) . . ? C35 C34 C39 118.7(4) . . ? C35 C34 P1 122.3(4) . . ? C39 C34 P1 118.9(4) . . ? C36 C35 C34 120.9(5) . . ? C37 C36 C35 119.9(6) . . ? C36 C37 C38 120.5(5) . . ? C37 C38 C39 119.5(6) . . ? C34 C39 C38 120.5(5) . . ? C45 C40 C41 118.5(4) . . ? C45 C40 P1 120.2(3) . . ? C41 C40 P1 121.3(3) . . ? C42 C41 C40 119.8(4) . . ? C43 C42 C41 121.1(4) . . ? C42 C43 C44 118.7(4) . . ? C45 C44 C43 121.1(4) . . ? C44 C45 C40 120.8(4) . . ? C47 C46 C51 118.8(4) . . ? C47 C46 P1 117.7(3) . . ? C51 C46 P1 123.4(4) . . ? C46 C47 C48 121.1(5) . . ? C49 C48 C47 120.2(6) . . ? C50 C49 C48 119.6(5) . . ? C49 C50 C51 120.5(5) . . ? C46 C51 C50 119.7(5) . . ? C57 C52 C53 118.6(4) . . ? C57 C52 P2 119.5(4) . . ? C53 C52 P2 121.8(4) . . ? C54 C53 C52 120.8(5) . . ? C55 C54 C53 119.3(6) . . ? C54 C55 C56 121.1(5) . . ? C57 C56 C55 119.1(5) . . ? C56 C57 C52 121.1(5) . . ? C63 C58 C59 118.3(4) . . ? C63 C58 P2 120.5(4) . . ? C59 C58 P2 120.6(4) . . ? C60 C59 C58 120.6(5) . . ? C61 C60 C59 120.0(5) . . ? C62 C61 C60 121.0(5) . . ? C61 C62 C63 120.4(6) . . ? C58 C63 C62 119.6(5) . . ? C65 C64 C69 118.4(4) . . ? C65 C64 P2 117.2(3) . . ? C69 C64 P2 124.0(4) . . ? C64 C65 C66 121.2(5) . . ? C67 C66 C65 119.1(6) . . ? C68 C67 C66 119.7(5) . . ? C67 C68 C69 121.7(5) . . ? C68 C69 C64 119.9(5) . . ? C75 C70 C71 118.5(5) . . ? C75 C70 P3 117.7(4) . . ? C71 C70 P3 123.8(4) . . ? C70 C71 C72 120.2(6) . . ? C73 C72 C71 121.7(6) . . ? C72 C73 C74 120.2(6) . . ? C73 C74 C75 118.8(6) . . ? C70 C75 C74 120.6(5) . . ? C77 C76 C81 118.9(4) . . ? C77 C76 P3 118.9(3) . . ? C81 C76 P3 122.2(3) . . ? C76 C77 C78 120.8(4) . . ? C79 C78 C77 118.6(5) . . ? C80 C79 C78 120.9(5) . . ? C79 C80 C81 120.7(5) . . ? C80 C81 C76 120.0(5) . . ? C83 C82 C87 117.1(4) . . ? C83 C82 P3 123.0(4) . . ? C87 C82 P3 119.6(3) . . ? C82 C83 C84 119.5(6) . . ? C85 C84 C83 121.7(6) . . ? C86 C85 C84 118.7(5) . . ? C85 C86 C87 120.9(6) . . ? C86 C87 C82 121.9(4) . . ? C93 C88 C89 119.2(4) . . ? C93 C88 P4 123.4(3) . . ? C89 C88 P4 117.3(3) . . ? C90 C89 C88 120.5(5) . . ? C89 C90 C91 119.7(5) . . ? C92 C91 C90 119.0(4) . . ? C91 C92 C93 122.0(5) . . ? C88 C93 C92 119.6(4) . . ? C99 C94 C96 118.5(4) . . ? C99 C94 P4 124.3(3) . . ? C96 C94 P4 116.8(3) . . ? C98 C95 C99 121.6(5) . . ? C97 C96 C94 120.2(4) . . ? C98 C97 C96 120.7(4) . . ? C95 C98 C97 118.9(5) . . ? C94 C99 C95 120.0(4) . . ? C105 C100 C101 118.2(4) . . ? C105 C100 P4 123.1(3) . . ? C101 C100 P4 118.8(3) . . ? C102 C101 C100 120.3(4) . . ? C101 C102 C103 121.0(4) . . ? C104 C103 C102 119.3(5) . . ? C103 C104 C105 121.0(5) . . ? C104 C105 C100 120.2(4) . . ? F5A F5 B2 65(2) . . ? F6A F6 B2 63.5(7) . . ? F7A F7 B2 69.4(10) . . ? F7 F7A B2 58.1(12) . . ? F6 F6A B2 65.6(8) . . ? F5 F5A B2 83(2) . . ? F4 B1 F3 111.0(4) . . ? F4 B1 F2 109.6(4) . . ? F3 B1 F2 110.7(4) . . ? F4 B1 F1 109.0(4) . . ? F3 B1 F1 109.0(4) . . ? F2 B1 F1 107.6(4) . . ? F5A B2 F6A 132.5(17) . . ? F5A B2 F6 89.0(13) . . ? F6A B2 F6 50.9(6) . . ? F5A B2 F7 126.5(14) . . ? F6A B2 F7 100.9(12) . . ? F6 B2 F7 137.9(11) . . ? F5A B2 F5 32.0(15) . . ? F6A B2 F5 154.1(11) . . ? F6 B2 F5 103.3(9) . . ? F7 B2 F5 99.7(8) . . ? F5A B2 F7A 127(2) . . ? F6A B2 F7A 82.2(12) . . ? F6 B2 F7A 89.3(11) . . ? F7 B2 F7A 52.5(11) . . ? F5 B2 F7A 98.2(14) . . ? F5A B2 F8 89.9(14) . . ? F6A B2 F8 88.0(8) . . ? F6 B2 F8 116.5(8) . . ? F7 B2 F8 88.5(7) . . ? F5 B2 F8 108.0(8) . . ? F7A B2 F8 136.4(16) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 0.541 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.071 # Attachment '5.cif' data_jli3 _database_code_depnum_ccdc_archive 'CCDC 699120' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H44 Ag3 N15 O11' _chemical_formula_weight 1426.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.138(11) _cell_length_b 9.961(4) _cell_length_c 19.959(8) _cell_angle_alpha 90.00 _cell_angle_beta 112.053(7) _cell_angle_gamma 90.00 _cell_volume 5369(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description thin _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856 _exptl_absorpt_coefficient_mu 1.162 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8008 _exptl_absorpt_correction_T_max 0.8926 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 P4' _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 13863 _diffrn_reflns_av_R_equivalents 0.1073 _diffrn_reflns_av_sigmaI/netI 0.1771 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5260 _reflns_number_gt 2169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1050P)^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 5260 _refine_ls_number_parameters 389 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2034 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.1794 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.63654(14) 0.2500 0.0540(5) Uani 1 2 d S . . Ag2 Ag -0.21987(4) 0.37268(9) 0.08629(6) 0.0458(4) Uani 1 1 d . . . N1 N -0.0239(4) 0.4150(10) 0.1132(6) 0.046(3) Uani 1 1 d . . . N2 N 0.0310(4) 0.5998(11) 0.1666(6) 0.053(3) Uani 1 1 d . . . N3 N -0.1215(4) 0.2407(10) 0.2426(6) 0.043(3) Uani 1 1 d . . . N4 N -0.2110(4) 0.2343(10) 0.1864(6) 0.042(3) Uani 1 1 d . . . N5 N -0.1561(4) 0.6849(9) 0.1363(6) 0.046(3) Uani 1 1 d . . . N6 N -0.2389(4) 0.5918(9) 0.0915(5) 0.040(3) Uani 1 1 d . . . N7 N -0.1699(4) 0.2492(11) -0.0089(7) 0.053(3) Uani 1 1 d . . . N8 N 0.0000 0.978(2) 0.2500 0.071(6) Uani 1 2 d S . . O1 O -0.1983(4) 0.2008(9) 0.0177(5) 0.069(3) Uani 1 1 d . . . O2 O -0.1572(4) 0.1805(9) -0.0497(6) 0.078(3) Uani 1 1 d . . . O3 O -0.1586(4) 0.3658(10) 0.0021(6) 0.083(3) Uani 1 1 d . . . O4 O -0.0173(10) 0.870(2) 0.2689(19) 0.127(11) Uani 0.50 1 d P . . O5 O -0.0206(5) 1.0326(14) 0.1935(7) 0.101(4) Uani 1 1 d . . . C1 C 0.0713(5) 0.6653(15) 0.1662(8) 0.067(4) Uani 1 1 d . . . H1A H 0.0819 0.7441 0.1945 0.080 Uiso 1 1 calc R . . C2 C 0.0973(6) 0.621(2) 0.1259(11) 0.088(6) Uani 1 1 d . . . H2A H 0.1243 0.6737 0.1252 0.105 Uiso 1 1 calc R . . C3 C 0.0864(7) 0.507(2) 0.0874(11) 0.087(6) Uani 1 1 d . . . H3A H 0.1072 0.4718 0.0646 0.105 Uiso 1 1 calc R . . C4 C 0.0430(6) 0.4433(19) 0.0829(9) 0.069(5) Uani 1 1 d . . . C5 C 0.0155(6) 0.3290(17) 0.0452(9) 0.074(5) Uani 1 1 d . . . H5A H 0.0237 0.2733 0.0126 0.089 Uiso 1 1 calc R . . C6 C -0.0235(6) 0.3147(14) 0.0639(8) 0.063(4) Uani 1 1 d . . . H6A H -0.0478 0.2461 0.0463 0.076 Uiso 1 1 calc R . . C7 C 0.0169(6) 0.4923(15) 0.1228(8) 0.056(4) Uani 1 1 d . . . C8 C -0.2511(6) 0.1667(13) 0.1875(8) 0.055(4) Uani 1 1 d . . . H8A H -0.2830 0.1932 0.1550 0.066 Uiso 1 1 calc R . . C9 C -0.2473(7) 0.0588(14) 0.2349(9) 0.068(5) Uani 1 1 d . . . H9A H -0.2766 0.0137 0.2324 0.082 Uiso 1 1 calc R . . C10 C -0.2038(7) 0.0177(15) 0.2833(8) 0.066(5) Uani 1 1 d . . . H10A H -0.2021 -0.0525 0.3163 0.079 Uiso 1 1 calc R . . C11 C -0.1606(6) 0.0821(11) 0.2837(7) 0.048(4) Uani 1 1 d . . . C12 C -0.1093(6) 0.0677(13) 0.3192(8) 0.060(4) Uani 1 1 d . . . H12A H -0.0931 0.0016 0.3545 0.072 Uiso 1 1 calc R . . C13 C -0.0860(6) 0.1654(12) 0.2945(8) 0.055(4) Uani 1 1 d . . . H13A H -0.0513 0.1787 0.3106 0.066 Uiso 1 1 calc R . . C14 C -0.1675(5) 0.1931(11) 0.2350(7) 0.043(3) Uani 1 1 d . . . C15 C -0.2880(5) 0.6288(12) 0.0626(7) 0.047(3) Uani 1 1 d . . . H15A H -0.3123 0.5602 0.0459 0.056 Uiso 1 1 calc R . . C16 C -0.3032(6) 0.7572(15) 0.0569(8) 0.067(4) Uani 1 1 d . . . H16A H -0.3376 0.7758 0.0414 0.080 Uiso 1 1 calc R . . C17 C -0.2699(7) 0.8630(13) 0.0730(7) 0.068(5) Uani 1 1 d . . . H17A H -0.2809 0.9535 0.0644 0.081 Uiso 1 1 calc R . . C18 C -0.2200(6) 0.8315(12) 0.1021(7) 0.049(4) Uani 1 1 d . . . C19 C -0.1770(5) 0.9075(12) 0.1218(7) 0.050(4) Uani 1 1 d . . . H19A H -0.1748 1.0027 0.1214 0.060 Uiso 1 1 calc R . . C20 C -0.1370(6) 0.8160(13) 0.1428(8) 0.062(4) Uani 1 1 d . . . H20A H -0.1030 0.8391 0.1586 0.074 Uiso 1 1 calc R . . C21 C -0.2081(4) 0.6940(11) 0.1099(6) 0.033(3) Uiso 1 1 d . . . C22 C -0.0619(5) 0.4335(12) 0.1409(7) 0.045(3) Uani 1 1 d . . . C23 C -0.0729(5) 0.3334(12) 0.1793(7) 0.047(3) Uani 1 1 d . . . H23A H -0.0538 0.2533 0.1895 0.056 Uiso 1 1 calc R . . C24 C -0.1113(4) 0.3467(10) 0.2036(7) 0.038(3) Uani 1 1 d . . . C25 C -0.1378(5) 0.4659(12) 0.1913(7) 0.042(3) Uani 1 1 d . . . C26 C -0.1271(5) 0.5676(11) 0.1535(7) 0.042(3) Uani 1 1 d . . . C27 C -0.0886(4) 0.5561(12) 0.1261(7) 0.045(3) Uani 1 1 d . . . H27A H -0.0812 0.6264 0.0996 0.055 Uiso 1 1 calc R . . C28 C 0.0718(6) 0.9476(15) 0.4731(9) 0.080(5) Uani 1 1 d . . . H28A H 0.0847 0.9202 0.5240 0.119 Uiso 1 1 calc R . . H28B H 0.0502 1.0258 0.4668 0.119 Uiso 1 1 calc R . . H28C H 0.0994 0.9709 0.4586 0.119 Uiso 1 1 calc R . . H25A H -0.167(5) 0.475(15) 0.198(8) 0.096 Uiso 1 1 d . . . O6 O 0.0446(5) 0.8411(11) 0.4300(7) 0.094(4) Uani 1 1 d D . . H6 H 0.0362 0.8615 0.3861 0.141 Uiso 1 1 calc RD . . 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 0.0574(10) 0.0472(8) 0.0624(12) 0.000 0.0282(9) 0.000 Ag2 0.0477(6) 0.0403(5) 0.0542(8) -0.0034(6) 0.0247(5) -0.0032(5) N1 0.040(7) 0.056(6) 0.050(8) -0.008(6) 0.027(6) -0.005(5) N2 0.046(7) 0.068(7) 0.048(8) 0.014(7) 0.023(6) -0.005(6) N3 0.050(7) 0.042(6) 0.042(7) 0.001(6) 0.022(6) -0.004(6) N4 0.051(7) 0.050(6) 0.036(7) -0.005(5) 0.028(6) -0.006(6) N5 0.067(8) 0.028(5) 0.050(8) -0.004(5) 0.029(6) -0.001(5) N6 0.056(7) 0.043(6) 0.033(6) 0.007(5) 0.030(6) 0.010(5) N7 0.047(7) 0.053(7) 0.069(10) -0.003(7) 0.035(7) -0.010(6) N8 0.082(17) 0.065(13) 0.065(17) 0.000 0.025(14) 0.000 O1 0.085(8) 0.069(6) 0.070(8) -0.023(6) 0.051(7) -0.018(6) O2 0.119(9) 0.052(5) 0.100(9) -0.018(6) 0.082(8) -0.009(6) O3 0.092(9) 0.058(6) 0.099(9) -0.019(7) 0.038(7) -0.017(6) O4 0.14(3) 0.050(12) 0.21(4) -0.014(17) 0.09(2) -0.018(14) O5 0.103(11) 0.125(11) 0.081(10) 0.000(9) 0.041(9) 0.009(9) C1 0.050(9) 0.094(11) 0.063(11) 0.000(9) 0.029(8) -0.026(9) C2 0.059(11) 0.119(15) 0.106(16) 0.055(14) 0.054(11) 0.022(12) C3 0.065(13) 0.109(14) 0.109(17) 0.037(13) 0.058(12) 0.041(12) C4 0.049(10) 0.102(13) 0.055(12) 0.017(10) 0.019(9) -0.003(10) C5 0.071(11) 0.107(13) 0.067(12) 0.031(11) 0.052(10) 0.044(11) C6 0.085(12) 0.055(8) 0.037(10) 0.001(8) 0.010(9) 0.005(8) C7 0.061(11) 0.069(9) 0.043(10) 0.016(8) 0.026(9) 0.010(9) C8 0.072(10) 0.060(8) 0.046(9) -0.008(7) 0.037(8) 0.001(8) C9 0.110(15) 0.059(9) 0.061(12) 0.005(9) 0.061(11) -0.031(9) C10 0.117(15) 0.063(9) 0.034(10) 0.011(8) 0.047(10) 0.000(10) C11 0.098(12) 0.036(6) 0.026(8) 0.016(6) 0.041(9) 0.016(8) C12 0.092(13) 0.043(8) 0.059(11) 0.005(7) 0.045(10) 0.022(8) C13 0.078(11) 0.041(7) 0.054(10) -0.008(7) 0.036(9) -0.012(7) C14 0.076(11) 0.027(6) 0.041(9) 0.003(6) 0.041(8) 0.009(7) C15 0.053(9) 0.051(7) 0.036(8) 0.007(7) 0.017(7) 0.008(7) C16 0.078(11) 0.066(10) 0.075(13) 0.000(9) 0.051(10) 0.017(9) C17 0.130(16) 0.040(8) 0.033(9) 0.010(7) 0.030(10) 0.023(10) C18 0.072(11) 0.032(6) 0.044(10) 0.010(6) 0.023(8) 0.007(7) C19 0.075(11) 0.039(7) 0.037(9) -0.006(6) 0.022(8) 0.012(8) C20 0.085(12) 0.041(7) 0.055(11) -0.013(7) 0.020(9) -0.021(8) C22 0.048(9) 0.043(7) 0.053(10) 0.008(7) 0.028(8) -0.001(6) C23 0.047(8) 0.040(7) 0.049(10) -0.005(7) 0.013(7) 0.008(6) C24 0.033(7) 0.032(6) 0.053(9) -0.001(6) 0.018(7) -0.014(6) C25 0.038(8) 0.046(7) 0.040(9) -0.003(7) 0.013(7) -0.004(7) C26 0.051(9) 0.024(6) 0.051(9) -0.002(6) 0.019(7) -0.006(6) C27 0.040(8) 0.051(7) 0.039(9) -0.002(7) 0.008(7) -0.008(6) C28 0.089(13) 0.073(10) 0.068(13) -0.028(9) 0.020(10) -0.028(10) O6 0.126(11) 0.089(8) 0.088(9) 0.012(7) 0.064(9) -0.029(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 N2 2.202(11) . ? Ag1 N2 2.202(11) 2 ? Ag1 O4 2.44(2) 2 ? Ag1 O4 2.44(2) . ? Ag2 N6 2.264(9) . ? Ag2 N4 2.360(10) . ? Ag2 O1 2.418(9) . ? Ag2 C25 2.684(13) . ? N1 C7 1.368(16) . ? N1 C6 1.405(16) . ? N1 C22 1.424(15) . ? N2 C7 1.344(17) . ? N2 C1 1.346(15) . ? N3 C14 1.375(15) . ? N3 C13 1.378(16) . ? N3 C24 1.409(14) . ? N4 C14 1.339(15) . ? N4 C8 1.355(15) . ? N5 C20 1.406(15) . ? N5 C21 1.407(14) . ? N5 C26 1.407(14) . ? N6 C21 1.317(14) . ? N6 C15 1.376(15) . ? N7 O3 1.205(12) . ? N7 O2 1.221(13) . ? N7 O1 1.238(12) . ? N8 O5 1.189(14) 2 ? N8 O5 1.189(14) . ? N8 O4 1.31(2) . ? N8 O4 1.31(2) 2 ? O4 O4 1.47(5) 2 ? C1 C2 1.37(2) . ? C2 C3 1.34(2) . ? C3 C4 1.39(2) . ? C4 C7 1.38(2) . ? C4 C5 1.43(2) . ? C5 C6 1.331(19) . ? C8 C9 1.410(18) . ? C9 C10 1.34(2) . ? C10 C11 1.41(2) . ? C11 C12 1.401(19) . ? C11 C14 1.436(16) . ? C12 C13 1.378(17) . ? C15 C16 1.344(16) . ? C16 C17 1.385(19) . ? C17 C18 1.386(19) . ? C18 C19 1.389(18) . ? C18 C21 1.406(15) . ? C19 C20 1.413(18) . ? C22 C23 1.368(16) . ? C22 C27 1.418(16) . ? C23 C24 1.382(16) . ? C24 C25 1.388(16) . ? C25 C26 1.369(16) . ? C26 C27 1.424(17) . ? C28 O6 1.407(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N2 160.8(6) . 2 ? N2 Ag1 O4 82.8(7) . 2 ? N2 Ag1 O4 116.3(8) 2 2 ? N2 Ag1 O4 116.3(8) . . ? N2 Ag1 O4 82.8(7) 2 . ? O4 Ag1 O4 35.1(12) 2 . ? N6 Ag2 N4 118.4(3) . . ? N6 Ag2 O1 146.0(3) . . ? N4 Ag2 O1 95.6(3) . . ? N6 Ag2 C25 78.0(4) . . ? N4 Ag2 C25 76.0(4) . . ? O1 Ag2 C25 110.1(4) . . ? C7 N1 C6 105.3(11) . . ? C7 N1 C22 129.4(11) . . ? C6 N1 C22 125.1(11) . . ? C7 N2 C1 115.8(13) . . ? C7 N2 Ag1 120.8(9) . . ? C1 N2 Ag1 122.0(10) . . ? C14 N3 C13 108.7(10) . . ? C14 N3 C24 126.6(11) . . ? C13 N3 C24 124.7(11) . . ? C14 N4 C8 115.0(11) . . ? C14 N4 Ag2 124.4(8) . . ? C8 N4 Ag2 118.8(9) . . ? C20 N5 C21 107.9(10) . . ? C20 N5 C26 124.6(11) . . ? C21 N5 C26 127.5(9) . . ? C21 N6 C15 113.8(10) . . ? C21 N6 Ag2 127.2(8) . . ? C15 N6 Ag2 118.2(8) . . ? O3 N7 O2 122.1(12) . . ? O3 N7 O1 118.5(12) . . ? O2 N7 O1 119.1(11) . . ? O5 N8 O5 126(2) 2 . ? O5 N8 O4 102.4(17) 2 . ? O5 N8 O4 122.4(19) . . ? O5 N8 O4 122.4(19) 2 2 ? O5 N8 O4 102.4(17) . 2 ? O4 N8 O4 68(2) . 2 ? N7 O1 Ag2 109.0(8) . . ? N8 O4 O4 55.8(12) . 2 ? N8 O4 Ag1 128.2(17) . . ? O4 O4 Ag1 72.5(6) 2 . ? N2 C1 C2 121.6(16) . . ? C3 C2 C1 123.1(17) . . ? C2 C3 C4 115.9(17) . . ? C7 C4 C3 119.2(18) . . ? C7 C4 C5 105.3(14) . . ? C3 C4 C5 135.6(18) . . ? C6 C5 C4 107.8(14) . . ? C5 C6 N1 110.6(14) . . ? N2 C7 N1 125.2(13) . . ? N2 C7 C4 123.9(15) . . ? N1 C7 C4 110.9(14) . . ? N4 C8 C9 122.6(14) . . ? C10 C9 C8 122.2(15) . . ? C9 C10 C11 117.9(14) . . ? C12 C11 C10 137.5(13) . . ? C12 C11 C14 105.8(13) . . ? C10 C11 C14 116.6(14) . . ? C13 C12 C11 108.7(13) . . ? N3 C13 C12 108.8(13) . . ? N4 C14 N3 126.3(11) . . ? N4 C14 C11 125.5(13) . . ? N3 C14 C11 107.9(13) . . ? C16 C15 N6 123.2(13) . . ? C15 C16 C17 121.7(14) . . ? C16 C17 C18 117.2(13) . . ? C17 C18 C19 133.6(12) . . ? C17 C18 C21 116.4(13) . . ? C19 C18 C21 109.9(13) . . ? C18 C19 C20 106.7(12) . . ? N5 C20 C19 108.6(13) . . ? N6 C21 C18 127.4(12) . . ? N6 C21 N5 125.5(10) . . ? C18 C21 N5 106.9(11) . . ? C23 C22 C27 121.3(11) . . ? C23 C22 N1 120.3(11) . . ? C27 C22 N1 118.4(11) . . ? C22 C23 C24 121.2(11) . . ? C23 C24 C25 119.4(11) . . ? C23 C24 N3 119.2(10) . . ? C25 C24 N3 121.3(11) . . ? C26 C25 C24 120.1(12) . . ? C26 C25 Ag2 98.4(9) . . ? C24 C25 Ag2 96.7(8) . . ? C25 C26 N5 120.5(11) . . ? C25 C26 C27 121.9(11) . . ? N5 C26 C27 117.4(11) . . ? C22 C27 C26 116.0(11) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.057 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.147 # Attachment '6.cif' data_jli1 _database_code_depnum_ccdc_archive 'CCDC 699121' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H30 Ag4 N22 O12' _chemical_formula_weight 1538.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.365(5) _cell_length_b 10.660(5) _cell_length_c 12.142(6) _cell_angle_alpha 100.933(8) _cell_angle_beta 94.262(8) _cell_angle_gamma 115.538(7) _cell_volume 1170.0(9) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 1.746 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7215 _exptl_absorpt_correction_T_max 0.8447 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7037 _diffrn_reflns_av_R_equivalents 0.0942 _diffrn_reflns_av_sigmaI/netI 0.2683 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4514 _reflns_number_gt 1796 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4514 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1821 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.847 _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 1.31854(10) 1.03317(10) 0.39678(10) 0.0483(4) Uani 1 1 d . . . Ag2 Ag 0.76686(10) 0.96726(10) 0.26600(9) 0.0421(3) Uani 1 1 d . . . O1 O 0.9672(9) 1.1427(9) 0.6168(9) 0.056(3) Uani 1 1 d . . . O2 O 0.8150(8) 1.0270(8) 0.4634(7) 0.045(2) Uani 1 1 d . . . O3 O 1.0388(10) 1.1684(9) 0.4589(8) 0.056(3) Uani 1 1 d . . . O4 O 1.5289(10) 0.9052(10) 0.3341(9) 0.091(4) Uani 1 1 d . . . O5 O 1.2998(10) 0.7934(9) 0.2999(8) 0.064(3) Uani 1 1 d . . . O6 O 1.4245(12) 0.7323(10) 0.1891(9) 0.079(4) Uani 1 1 d . . . N1 N 1.2404(10) 1.1522(10) 0.2557(8) 0.038(3) Uani 1 1 d . . . N2 N 1.0021(10) 1.1223(10) 0.1935(8) 0.029(3) Uani 1 1 d . . . N3 N 1.1940(9) 1.3515(9) 0.2878(7) 0.025(2) Uani 1 1 d . . . N4 N 1.4231(9) 1.3805(9) 0.3379(8) 0.031(2) Uani 1 1 d . . . N5 N 1.5184(9) 1.2277(9) 0.3991(8) 0.037(3) Uani 1 1 d . . . N6 N 1.0596(10) 0.9360(9) 0.1509(8) 0.030(2) Uani 1 1 d . . . N7 N 0.7966(10) 0.8234(10) 0.1171(8) 0.036(3) Uani 1 1 d . . . N8 N 0.9660(9) 1.3251(9) 0.2337(8) 0.026(2) Uani 1 1 d . . . N9 N 0.7247(10) 1.1255(10) 0.1784(8) 0.034(3) Uani 1 1 d . . . N10 N 0.9438(13) 1.1152(11) 0.5143(11) 0.037(3) Uani 1 1 d . . . C1 C 1.2781(12) 1.2900(13) 0.2922(10) 0.034(3) Uani 1 1 d . . . C2 C 1.1002(12) 1.0751(11) 0.2070(10) 0.031(3) Uani 1 1 d . . . C3 C 1.0574(13) 1.2660(13) 0.2412(9) 0.032(3) Uani 1 1 d . . . C4 C 1.4840(12) 1.5277(12) 0.3418(11) 0.040(3) Uani 1 1 d . . . H4A H 1.4330 1.5758 0.3169 0.048 Uiso 1 1 calc R . . C5 C 1.6229(14) 1.5878(13) 0.3855(11) 0.049(4) Uani 1 1 d . . . H5A H 1.6887 1.6864 0.3964 0.059 Uiso 1 1 calc R . . C6 C 1.6587(11) 1.4842(12) 0.4133(11) 0.039(4) Uani 1 1 d . . . C7 C 1.7808(13) 1.4822(13) 0.4618(10) 0.043(4) Uani 1 1 d . . . H7A H 1.8697 1.5678 0.4868 0.052 Uiso 1 1 calc R . . C8 C 1.7716(12) 1.3518(13) 0.4735(10) 0.038(3) Uani 1 1 d . . . H8A H 1.8567 1.3463 0.5012 0.046 Uiso 1 1 calc R . . C9 C 1.6424(14) 1.2326(13) 0.4456(10) 0.047(4) Uani 1 1 d . . . H9A H 1.6392 1.1468 0.4599 0.056 Uiso 1 1 calc R . . C10 C 1.5323(12) 1.3546(12) 0.3832(10) 0.036(3) Uani 1 1 d . . . C11 C 1.1551(13) 0.8835(14) 0.1232(11) 0.042(4) Uani 1 1 d . . . H11A H 1.2567 0.9350 0.1510 0.050 Uiso 1 1 calc R . . C12 C 1.0923(13) 0.7544(13) 0.0543(11) 0.041(3) Uani 1 1 d . . . H12A H 1.1390 0.6998 0.0231 0.050 Uiso 1 1 calc R . . C13 C 0.9404(14) 0.7124(13) 0.0355(10) 0.038(3) Uani 1 1 d . . . C14 C 0.8173(15) 0.5928(12) -0.0278(10) 0.048(4) Uani 1 1 d . . . H14A H 0.8226 0.5130 -0.0737 0.058 Uiso 1 1 calc R . . C15 C 0.6862(13) 0.5965(12) -0.0202(10) 0.040(3) Uani 1 1 d . . . H15A H 0.5988 0.5212 -0.0660 0.048 Uiso 1 1 calc R . . C16 C 0.6829(13) 0.7089(14) 0.0535(11) 0.046(4) Uani 1 1 d . . . H16A H 0.5901 0.7041 0.0594 0.055 Uiso 1 1 calc R . . C17 C 0.9200(13) 0.8263(12) 0.0994(10) 0.035(3) Uani 1 1 d . . . C18 C 1.0197(13) 1.4744(11) 0.2526(10) 0.036(3) Uani 1 1 d . . . H18A H 1.1178 1.5434 0.2817 0.043 Uiso 1 1 calc R . . C19 C 0.9096(12) 1.5040(12) 0.2227(10) 0.041(3) Uani 1 1 d . . . H19A H 0.9172 1.5969 0.2268 0.049 Uiso 1 1 calc R . . C20 C 0.7805(13) 1.3724(12) 0.1840(9) 0.034(3) Uani 1 1 d . . . C21 C 0.6377(11) 1.3351(12) 0.1409(11) 0.039(3) Uani 1 1 d . . . H21A H 0.6079 1.4046 0.1282 0.047 Uiso 1 1 calc R . . C22 C 0.5426(12) 1.1932(13) 0.1179(10) 0.039(3) Uani 1 1 d . . . H22A H 0.4433 1.1622 0.0888 0.047 Uiso 1 1 calc R . . C23 C 0.5889(13) 1.0921(12) 0.1363(10) 0.041(3) Uani 1 1 d . . . H23A H 0.5190 0.9940 0.1176 0.049 Uiso 1 1 calc R . . C24 C 0.8173(12) 1.2635(12) 0.1949(10) 0.031(3) Uani 1 1 d . . . N11 N 1.4180(13) 0.8075(11) 0.2720(10) 0.039(3) 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 0.0406(7) 0.0397(7) 0.0704(9) 0.0297(6) 0.0116(6) 0.0166(6) Ag2 0.0384(7) 0.0308(6) 0.0563(8) 0.0125(6) 0.0113(6) 0.0139(5) O1 0.061(6) 0.041(6) 0.039(7) -0.008(5) 0.009(6) 0.007(5) O2 0.031(5) 0.043(5) 0.042(6) -0.006(5) -0.016(4) 0.010(4) O3 0.063(6) 0.043(5) 0.061(7) 0.024(5) 0.016(5) 0.017(5) O4 0.058(7) 0.053(6) 0.099(9) -0.011(7) 0.008(6) -0.020(6) O5 0.046(6) 0.057(6) 0.082(8) 0.030(6) 0.007(6) 0.013(5) O6 0.127(10) 0.043(6) 0.076(8) 0.005(6) 0.033(7) 0.048(7) N1 0.036(6) 0.033(6) 0.038(7) 0.001(5) -0.006(5) 0.017(5) N2 0.033(6) 0.033(6) 0.029(7) 0.004(5) 0.015(5) 0.021(5) N3 0.021(5) 0.019(5) 0.029(6) 0.004(5) -0.007(5) 0.007(5) N4 0.023(5) 0.022(5) 0.042(7) 0.011(5) -0.008(5) 0.006(4) N5 0.027(6) 0.025(6) 0.052(7) 0.009(5) -0.003(5) 0.009(5) N6 0.034(6) 0.027(6) 0.031(6) 0.011(5) 0.003(5) 0.014(5) N7 0.023(6) 0.035(6) 0.053(8) 0.011(5) 0.001(5) 0.016(5) N8 0.025(5) 0.020(5) 0.035(6) 0.004(5) -0.007(5) 0.014(4) N9 0.029(6) 0.031(6) 0.040(7) 0.006(5) 0.004(5) 0.013(5) N10 0.063(9) 0.023(6) 0.034(8) 0.007(6) 0.015(7) 0.026(6) C1 0.027(7) 0.036(8) 0.025(8) 0.002(6) -0.009(6) 0.008(6) C2 0.027(7) 0.021(6) 0.040(9) 0.004(6) 0.005(6) 0.009(6) C3 0.045(8) 0.039(8) 0.013(7) 0.002(6) -0.006(6) 0.023(7) C4 0.026(7) 0.030(7) 0.072(11) 0.023(7) 0.012(7) 0.016(6) C5 0.055(10) 0.026(7) 0.063(11) 0.019(7) 0.005(8) 0.012(7) C6 0.014(6) 0.025(7) 0.062(10) -0.001(7) -0.013(6) 0.002(5) C7 0.039(8) 0.033(8) 0.037(9) -0.011(7) -0.003(7) 0.006(6) C8 0.026(7) 0.044(8) 0.039(9) -0.008(7) -0.011(6) 0.021(7) C9 0.057(9) 0.035(8) 0.045(10) 0.000(7) -0.009(8) 0.024(7) C10 0.035(7) 0.034(7) 0.051(9) 0.029(7) 0.018(7) 0.017(6) C11 0.029(7) 0.052(9) 0.047(10) 0.011(8) 0.013(7) 0.020(7) C12 0.049(9) 0.038(8) 0.048(10) 0.010(7) 0.025(7) 0.027(7) C13 0.056(9) 0.043(8) 0.036(9) 0.030(7) 0.018(7) 0.032(7) C14 0.069(10) 0.023(7) 0.034(9) 0.008(6) 0.005(8) 0.003(7) C15 0.034(8) 0.026(7) 0.034(9) -0.005(7) -0.012(7) -0.003(6) C16 0.041(8) 0.052(9) 0.052(10) 0.019(8) -0.009(7) 0.028(7) C17 0.043(8) 0.033(7) 0.028(8) 0.004(6) 0.000(7) 0.019(7) C18 0.039(7) 0.016(6) 0.033(8) -0.004(6) -0.014(6) 0.002(6) C19 0.043(8) 0.013(6) 0.052(9) -0.005(6) -0.011(7) 0.008(6) C20 0.056(9) 0.047(8) 0.019(8) 0.019(6) 0.014(6) 0.038(7) C21 0.023(7) 0.038(8) 0.074(11) 0.037(7) 0.010(7) 0.019(6) C22 0.027(7) 0.048(8) 0.049(10) 0.020(7) 0.006(7) 0.020(7) C23 0.035(8) 0.026(7) 0.040(9) 0.007(6) 0.001(7) -0.005(6) C24 0.034(7) 0.032(7) 0.026(8) -0.001(6) 0.008(6) 0.016(6) N11 0.053(8) 0.027(6) 0.048(9) 0.023(6) 0.011(7) 0.022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N5 2.204(9) . ? Ag1 O2 2.282(9) 2_776 ? Ag1 O5 2.520(9) . ? Ag1 N1 2.589(10) . ? Ag2 N7 2.271(9) . ? Ag2 O2 2.318(8) . ? Ag2 N9 2.327(10) . ? Ag2 O4 2.511(10) 1_455 ? Ag2 N2 2.617(9) . ? O1 N10 1.203(12) . ? O2 N10 1.274(12) . ? O2 Ag1 2.282(9) 2_776 ? O3 N10 1.227(12) . ? O4 N11 1.231(12) . ? O4 Ag2 2.511(10) 1_655 ? O5 N11 1.249(12) . ? O6 N11 1.188(12) . ? N1 C1 1.318(13) . ? N1 C2 1.340(12) . ? N2 C2 1.327(12) . ? N2 C3 1.367(13) . ? N3 C1 1.301(13) . ? N3 C3 1.315(13) . ? N4 C10 1.377(13) . ? N4 C1 1.385(13) . ? N4 C4 1.405(13) . ? N5 C9 1.340(14) . ? N5 C10 1.350(13) . ? N6 C11 1.364(13) . ? N6 C2 1.370(13) . ? N6 C17 1.408(13) . ? N7 C17 1.301(13) . ? N7 C16 1.320(13) . ? N8 C3 1.351(13) . ? N8 C24 1.389(13) . ? N8 C18 1.405(12) . ? N9 C23 1.327(13) . ? N9 C24 1.329(13) . ? C4 C5 1.314(15) . ? C5 C6 1.395(15) . ? C6 C7 1.367(15) . ? C6 C10 1.391(14) . ? C7 C8 1.387(16) . ? C8 C9 1.351(15) . ? C11 C12 1.315(14) . ? C12 C13 1.426(15) . ? C13 C14 1.387(15) . ? C13 C17 1.417(15) . ? C14 C15 1.386(16) . ? C15 C16 1.367(15) . ? C18 C19 1.352(14) . ? C19 C20 1.420(14) . ? C20 C21 1.386(14) . ? C20 C24 1.393(15) . ? C21 C22 1.360(14) . ? C22 C23 1.400(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ag1 O2 130.5(3) . 2_776 ? N5 Ag1 O5 118.2(3) . . ? O2 Ag1 O5 100.9(3) 2_776 . ? N5 Ag1 N1 75.5(3) . . ? O2 Ag1 N1 117.8(3) 2_776 . ? O5 Ag1 N1 112.5(3) . . ? N7 Ag2 O2 139.2(3) . . ? N7 Ag2 N9 101.8(3) . . ? O2 Ag2 N9 117.1(3) . . ? N7 Ag2 O4 123.2(3) . 1_455 ? O2 Ag2 O4 72.4(3) . 1_455 ? N9 Ag2 O4 88.2(4) . 1_455 ? N7 Ag2 N2 71.8(3) . . ? O2 Ag2 N2 108.4(3) . . ? N9 Ag2 N2 71.1(3) . . ? O4 Ag2 N2 157.3(3) 1_455 . ? N10 O2 Ag1 106.1(8) . 2_776 ? N10 O2 Ag2 118.6(8) . . ? Ag1 O2 Ag2 135.3(4) 2_776 . ? N11 O4 Ag2 118.3(9) . 1_655 ? N11 O5 Ag1 110.6(7) . . ? C1 N1 C2 112.6(10) . . ? C1 N1 Ag1 116.7(8) . . ? C2 N1 Ag1 112.2(7) . . ? C2 N2 C3 112.1(9) . . ? C2 N2 Ag2 110.4(7) . . ? C3 N2 Ag2 113.1(7) . . ? C1 N3 C3 115.8(9) . . ? C10 N4 C1 131.7(10) . . ? C10 N4 C4 107.2(9) . . ? C1 N4 C4 121.1(10) . . ? C9 N5 C10 114.0(10) . . ? C9 N5 Ag1 115.7(8) . . ? C10 N5 Ag1 128.7(8) . . ? C11 N6 C2 124.0(10) . . ? C11 N6 C17 106.6(9) . . ? C2 N6 C17 129.0(10) . . ? C17 N7 C16 113.3(10) . . ? C17 N7 Ag2 125.2(8) . . ? C16 N7 Ag2 120.1(8) . . ? C3 N8 C24 131.4(9) . . ? C3 N8 C18 120.8(9) . . ? C24 N8 C18 107.3(9) . . ? C23 N9 C24 114.2(10) . . ? C23 N9 Ag2 118.6(8) . . ? C24 N9 Ag2 124.3(8) . . ? O1 N10 O3 122.4(12) . . ? O1 N10 O2 117.6(12) . . ? O3 N10 O2 120.0(12) . . ? N3 C1 N1 126.9(10) . . ? N3 C1 N4 115.8(10) . . ? N1 C1 N4 117.2(11) . . ? N2 C2 N1 127.6(10) . . ? N2 C2 N6 116.2(10) . . ? N1 C2 N6 115.5(10) . . ? N3 C3 N8 118.0(10) . . ? N3 C3 N2 124.8(11) . . ? N8 C3 N2 117.1(10) . . ? C5 C4 N4 108.9(11) . . ? C4 C5 C6 109.3(11) . . ? C7 C6 C10 116.8(12) . . ? C7 C6 C5 136.1(11) . . ? C10 C6 C5 107.0(10) . . ? C6 C7 C8 118.3(11) . . ? C9 C8 C7 120.4(11) . . ? N5 C9 C8 124.2(12) . . ? N5 C10 N4 126.3(10) . . ? N5 C10 C6 126.2(11) . . ? N4 C10 C6 107.5(10) . . ? C12 C11 N6 113.2(11) . . ? C11 C12 C13 106.5(11) . . ? C14 C13 C17 117.2(12) . . ? C14 C13 C12 135.5(13) . . ? C17 C13 C12 107.3(11) . . ? C15 C14 C13 116.1(12) . . ? C16 C15 C14 119.8(11) . . ? N7 C16 C15 126.1(12) . . ? N7 C17 N6 126.7(11) . . ? N7 C17 C13 126.6(11) . . ? N6 C17 C13 106.3(10) . . ? C19 C18 N8 109.1(9) . . ? C18 C19 C20 108.2(10) . . ? C21 C20 C24 118.5(11) . . ? C21 C20 C19 134.5(11) . . ? C24 C20 C19 107.0(10) . . ? C22 C21 C20 116.2(11) . . ? C21 C22 C23 121.1(11) . . ? N9 C23 C22 123.8(10) . . ? N9 C24 N8 125.7(11) . . ? N9 C24 C20 125.8(11) . . ? N8 C24 C20 108.3(10) . . ? O6 N11 O4 121.0(13) . . ? O6 N11 O5 122.3(13) . . ? O4 N11 O5 116.7(12) . . ? 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 N7 Ag2 O2 N10 78.6(9) . . . . ? N9 Ag2 O2 N10 -82.2(8) . . . . ? O4 Ag2 O2 N10 -160.6(8) 1_455 . . . ? N2 Ag2 O2 N10 -4.5(8) . . . . ? N7 Ag2 O2 Ag1 -102.2(6) . . . 2_776 ? N9 Ag2 O2 Ag1 97.0(5) . . . 2_776 ? O4 Ag2 O2 Ag1 18.5(5) 1_455 . . 2_776 ? N2 Ag2 O2 Ag1 174.7(4) . . . 2_776 ? N5 Ag1 O5 N11 7.7(9) . . . . ? O2 Ag1 O5 N11 -140.8(8) 2_776 . . . ? N1 Ag1 O5 N11 92.8(8) . . . . ? N5 Ag1 N1 C1 -49.6(9) . . . . ? O2 Ag1 N1 C1 78.8(9) 2_776 . . . ? O5 Ag1 N1 C1 -164.5(8) . . . . ? N5 Ag1 N1 C2 178.3(8) . . . . ? O2 Ag1 N1 C2 -53.3(8) 2_776 . . . ? O5 Ag1 N1 C2 63.4(8) . . . . ? N7 Ag2 N2 C2 -63.3(7) . . . . ? O2 Ag2 N2 C2 73.7(7) . . . . ? N9 Ag2 N2 C2 -173.2(8) . . . . ? O4 Ag2 N2 C2 161.9(8) 1_455 . . . ? N7 Ag2 N2 C3 170.1(8) . . . . ? O2 Ag2 N2 C3 -52.9(8) . . . . ? N9 Ag2 N2 C3 60.2(8) . . . . ? O4 Ag2 N2 C3 35.3(13) 1_455 . . . ? O2 Ag1 N5 C9 80.7(9) 2_776 . . . ? O5 Ag1 N5 C9 -56.8(9) . . . . ? N1 Ag1 N5 C9 -164.9(9) . . . . ? O2 Ag1 N5 C10 -83.6(11) 2_776 . . . ? O5 Ag1 N5 C10 138.9(10) . . . . ? N1 Ag1 N5 C10 30.8(10) . . . . ? O2 Ag2 N7 C17 -56.3(11) . . . . ? N9 Ag2 N7 C17 106.2(10) . . . . ? O4 Ag2 N7 C17 -158.2(9) 1_455 . . . ? N2 Ag2 N7 C17 40.9(9) . . . . ? O2 Ag2 N7 C16 109.7(9) . . . . ? N9 Ag2 N7 C16 -87.7(9) . . . . ? O4 Ag2 N7 C16 7.8(10) 1_455 . . . ? N2 Ag2 N7 C16 -153.1(9) . . . . ? N7 Ag2 N9 C23 90.0(9) . . . . ? O2 Ag2 N9 C23 -102.6(8) . . . . ? O4 Ag2 N9 C23 -33.5(8) 1_455 . . . ? N2 Ag2 N9 C23 155.9(9) . . . . ? N7 Ag2 N9 C24 -110.4(9) . . . . ? O2 Ag2 N9 C24 57.0(10) . . . . ? O4 Ag2 N9 C24 126.1(9) 1_455 . . . ? N2 Ag2 N9 C24 -44.5(9) . . . . ? Ag1 O2 N10 O1 2.0(12) 2_776 . . . ? Ag2 O2 N10 O1 -178.6(8) . . . . ? Ag1 O2 N10 O3 -178.2(8) 2_776 . . . ? Ag2 O2 N10 O3 1.2(13) . . . . ? C3 N3 C1 N1 -0.5(19) . . . . ? C3 N3 C1 N4 177.9(10) . . . . ? C2 N1 C1 N3 2.2(19) . . . . ? Ag1 N1 C1 N3 -129.7(12) . . . . ? C2 N1 C1 N4 -176.2(10) . . . . ? Ag1 N1 C1 N4 51.9(13) . . . . ? C10 N4 C1 N3 160.2(12) . . . . ? C4 N4 C1 N3 -21.2(17) . . . . ? C10 N4 C1 N1 -21.2(19) . . . . ? C4 N4 C1 N1 157.4(11) . . . . ? C3 N2 C2 N1 -2.9(17) . . . . ? Ag2 N2 C2 N1 -130.1(11) . . . . ? C3 N2 C2 N6 -172.8(10) . . . . ? Ag2 N2 C2 N6 60.0(11) . . . . ? C1 N1 C2 N2 -0.2(18) . . . . ? Ag1 N1 C2 N2 133.9(11) . . . . ? C1 N1 C2 N6 169.7(10) . . . . ? Ag1 N1 C2 N6 -56.2(12) . . . . ? C11 N6 C2 N2 157.5(11) . . . . ? C17 N6 C2 N2 -14.2(18) . . . . ? C11 N6 C2 N1 -13.6(17) . . . . ? C17 N6 C2 N1 174.6(10) . . . . ? C1 N3 C3 N8 -179.4(11) . . . . ? C1 N3 C3 N2 -3.3(18) . . . . ? C24 N8 C3 N3 -176.4(11) . . . . ? C18 N8 C3 N3 13.1(16) . . . . ? C24 N8 C3 N2 7.2(19) . . . . ? C18 N8 C3 N2 -163.2(10) . . . . ? C2 N2 C3 N3 4.8(17) . . . . ? Ag2 N2 C3 N3 130.5(10) . . . . ? C2 N2 C3 N8 -179.1(10) . . . . ? Ag2 N2 C3 N8 -53.4(12) . . . . ? C10 N4 C4 C5 0.9(14) . . . . ? C1 N4 C4 C5 -178.1(11) . . . . ? N4 C4 C5 C6 -0.8(16) . . . . ? C4 C5 C6 C7 -178.4(14) . . . . ? C4 C5 C6 C10 0.4(16) . . . . ? C10 C6 C7 C8 2.4(18) . . . . ? C5 C6 C7 C8 -179.0(15) . . . . ? C6 C7 C8 C9 -5.1(19) . . . . ? C10 N5 C9 C8 -0.9(18) . . . . ? Ag1 N5 C9 C8 -167.5(10) . . . . ? C7 C8 C9 N5 4(2) . . . . ? C9 N5 C10 N4 -179.6(11) . . . . ? Ag1 N5 C10 N4 -15.1(18) . . . . ? C9 N5 C10 C6 -2.0(19) . . . . ? Ag1 N5 C10 C6 162.5(9) . . . . ? C1 N4 C10 N5 -4(2) . . . . ? C4 N4 C10 N5 177.4(11) . . . . ? C1 N4 C10 C6 178.2(12) . . . . ? C4 N4 C10 C6 -0.6(14) . . . . ? C7 C6 C10 N5 1.2(19) . . . . ? C5 C6 C10 N5 -177.8(12) . . . . ? C7 C6 C10 N4 179.2(10) . . . . ? C5 C6 C10 N4 0.2(15) . . . . ? C2 N6 C11 C12 -169.9(11) . . . . ? C17 N6 C11 C12 3.5(14) . . . . ? N6 C11 C12 C13 -1.9(15) . . . . ? C11 C12 C13 C14 179.2(13) . . . . ? C11 C12 C13 C17 -0.4(14) . . . . ? C17 C13 C14 C15 -1.1(16) . . . . ? C12 C13 C14 C15 179.3(13) . . . . ? C13 C14 C15 C16 -4.8(18) . . . . ? C17 N7 C16 C15 3.9(18) . . . . ? Ag2 N7 C16 C15 -163.7(10) . . . . ? C14 C15 C16 N7 4(2) . . . . ? C16 N7 C17 N6 177.6(11) . . . . ? Ag2 N7 C17 N6 -15.5(17) . . . . ? C16 N7 C17 C13 -10.8(18) . . . . ? Ag2 N7 C17 C13 156.0(9) . . . . ? C11 N6 C17 N7 169.4(12) . . . . ? C2 N6 C17 N7 -17.7(19) . . . . ? C11 N6 C17 C13 -3.5(12) . . . . ? C2 N6 C17 C13 169.4(11) . . . . ? C14 C13 C17 N7 9.8(18) . . . . ? C12 C13 C17 N7 -170.5(12) . . . . ? C14 C13 C17 N6 -177.2(10) . . . . ? C12 C13 C17 N6 2.4(13) . . . . ? C3 N8 C18 C19 170.4(11) . . . . ? C24 N8 C18 C19 -2.1(13) . . . . ? N8 C18 C19 C20 0.3(14) . . . . ? C18 C19 C20 C21 -178.2(13) . . . . ? C18 C19 C20 C24 1.6(14) . . . . ? C24 C20 C21 C22 3.2(17) . . . . ? C19 C20 C21 C22 -177.0(13) . . . . ? C20 C21 C22 C23 -0.5(18) . . . . ? C24 N9 C23 C22 -4.4(17) . . . . ? Ag2 N9 C23 C22 157.2(9) . . . . ? C21 C22 C23 N9 1(2) . . . . ? C23 N9 C24 N8 -177.4(10) . . . . ? Ag2 N9 C24 N8 22.2(16) . . . . ? C23 N9 C24 C20 7.5(18) . . . . ? Ag2 N9 C24 C20 -152.9(10) . . . . ? C3 N8 C24 N9 16(2) . . . . ? C18 N8 C24 N9 -172.8(11) . . . . ? C3 N8 C24 C20 -168.3(12) . . . . ? C18 N8 C24 C20 3.1(13) . . . . ? C21 C20 C24 N9 -7.2(19) . . . . ? C19 C20 C24 N9 173.0(12) . . . . ? C21 C20 C24 N8 176.9(10) . . . . ? C19 C20 C24 N8 -2.9(14) . . . . ? Ag2 O4 N11 O6 9.5(15) 1_655 . . . ? Ag2 O4 N11 O5 -169.6(8) 1_655 . . . ? Ag1 O5 N11 O6 -147.1(10) . . . . ? Ag1 O5 N11 O4 32.0(12) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.104 _refine_diff_density_min -1.176 _refine_diff_density_rms 0.153 # Attachment '7.cif' data_ew7 _database_code_depnum_ccdc_archive 'CCDC 699122' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H31 Ag4 N13 O13' _chemical_formula_weight 1297.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.0865(3) _cell_length_b 17.9907(4) _cell_length_c 15.2317(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.2810(10) _cell_angle_gamma 90.00 _cell_volume 4134.09(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3877 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.64 _exptl_crystal_description block _exptl_crystal_colour clear _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 1.951 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5922 _exptl_absorpt_correction_T_max 0.6963 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8043 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5738 _reflns_number_gt 5451 _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^)+(0.0570P)^2^+59.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.26(5) _refine_ls_number_reflns 5738 _refine_ls_number_parameters 607 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.65471(5) 0.29713(4) 2.20359(5) 0.0360(2) Uani 1 1 d . . . Ag2 Ag 0.34662(5) 0.30795(4) 1.97934(5) 0.0317(2) Uani 1 1 d . . . Ag3 Ag 0.51064(6) 0.16900(5) 2.48036(6) 0.0438(2) Uani 1 1 d . . . Ag4 Ag 0.48858(8) 0.22762(10) 1.72675(8) 0.0766(5) Uani 1 1 d . . . N1 N 0.6540(6) 0.4071(4) 2.1280(6) 0.029(2) Uani 1 1 d . . . N2 N 0.3503(5) 0.4136(4) 2.0662(6) 0.0235(17) Uani 1 1 d . . . N3 N 0.5024(6) 0.4098(4) 2.0966(7) 0.0246(16) Uani 1 1 d . . . N4 N 0.6384(5) 0.1858(4) 2.2743(5) 0.0195(17) Uani 1 1 d . . . N5 N 0.3990(5) 0.1586(5) 2.3822(6) 0.031(2) Uani 1 1 d . . . N6 N 0.3314(6) 0.2519(5) 1.6224(7) 0.035(2) Uani 1 1 d . . . N7 N 0.4828(5) 0.1773(4) 2.2544(6) 0.0245(18) Uani 1 1 d . . . N8 N 0.3572(6) 0.1887(4) 1.9184(6) 0.0262(19) Uani 1 1 d . . . N9 N 0.5940(6) 0.1691(6) 1.8040(6) 0.036(2) Uani 1 1 d . . . N10 N 0.5107(6) 0.1781(5) 1.9325(6) 0.0283(19) Uani 1 1 d . . . N11 N 0.6644(6) 0.2431(5) 2.5575(6) 0.033(2) Uani 1 1 d . . . N12 N 0.4935(7) 0.0397(5) 2.6070(6) 0.037(2) Uani 1 1 d . . . N13 N 0.4706(9) 0.3977(9) 1.8318(10) 0.066(4) Uani 1 1 d . . . O1 O 0.5916(6) 0.2604(6) 2.5863(6) 0.062(3) Uani 1 1 d . . . O2 O 0.6681(7) 0.2004(4) 2.4921(7) 0.047(2) Uani 1 1 d . . . O3 O 0.7326(6) 0.2669(5) 2.5897(6) 0.051(2) Uani 1 1 d . . . O4 O 0.4581(9) 0.1020(5) 2.6102(7) 0.079(4) Uani 1 1 d . . . O5 O 0.5397(11) 0.0242(8) 2.5446(9) 0.111(6) Uani 1 1 d . . . O6 O 0.4807(9) -0.0056(5) 2.6642(6) 0.074(4) Uani 1 1 d . . . O7 O 0.3293(6) 0.2198(5) 1.6966(6) 0.044(2) Uani 1 1 d . . . O8 O 0.4039(6) 0.2727(5) 1.5924(8) 0.062(3) Uani 1 1 d . . . O9 O 0.2608(6) 0.2643(6) 1.5855(7) 0.059(3) Uani 1 1 d . . . O10 O 0.4484(9) 0.4540(9) 1.8721(8) 0.085(4) Uani 1 1 d . . . O11 O 0.4275(7) 0.3423(7) 1.8295(7) 0.070(3) Uani 1 1 d . . . O12 O 0.5436(8) 0.4056(13) 1.7942(13) 0.169(10) Uani 1 1 d . . . O13 O 0.5363(16) 0.6016(8) 1.8357(10) 0.134(8) Uani 1 1 d . . . H13 H 0.5316 0.5575 1.8482 0.201 Uiso 1 1 calc R . . C1 C 0.5856(7) 0.4445(5) 2.0946(7) 0.023(2) Uani 1 1 d . . . C2 C 0.5954(8) 0.5153(6) 2.0566(8) 0.039(3) Uani 1 1 d . . . H2A H 0.5473 0.5402 2.0320 0.046 Uiso 1 1 calc R . . C3 C 0.6787(8) 0.5463(6) 2.0572(9) 0.041(3) Uani 1 1 d . . . H3A H 0.6865 0.5940 2.0351 0.049 Uiso 1 1 calc R . . C4 C 0.7491(8) 0.5092(6) 2.0888(9) 0.043(3) Uani 1 1 d . . . H4A H 0.8054 0.5303 2.0877 0.051 Uiso 1 1 calc R . . C5 C 0.7358(7) 0.4377(6) 2.1236(8) 0.033(2) Uani 1 1 d . . . H5A H 0.7843 0.4108 2.1441 0.040 Uiso 1 1 calc R . . C6 C 0.4214(8) 0.4481(6) 2.1001(8) 0.032(2) Uani 1 1 d . . . C7 C 0.4158(8) 0.5159(6) 2.1419(8) 0.036(3) Uani 1 1 d . . . H7A H 0.4661 0.5378 2.1662 0.044 Uiso 1 1 calc R . . C8 C 0.3356(8) 0.5504(7) 2.1472(9) 0.044(3) Uani 1 1 d . . . H8A H 0.3308 0.5969 2.1735 0.053 Uiso 1 1 calc R . . C9 C 0.2602(8) 0.5150(6) 2.1125(9) 0.043(3) Uani 1 1 d . . . H9A H 0.2047 0.5372 2.1159 0.052 Uiso 1 1 calc R . . C10 C 0.2704(8) 0.4467(6) 2.0732(8) 0.038(3) Uani 1 1 d . . . H10A H 0.2207 0.4226 2.0508 0.046 Uiso 1 1 calc R . . C11 C 0.5619(6) 0.1479(5) 2.2874(7) 0.025(2) Uani 1 1 d . . . C12 C 0.5629(7) 0.0803(5) 2.3323(8) 0.031(2) Uani 1 1 d . . . H12A H 0.5103 0.0551 2.3436 0.037 Uiso 1 1 calc R . . C13 C 0.6429(8) 0.0514(6) 2.3598(8) 0.035(3) Uani 1 1 d . . . H13A H 0.6445 0.0063 2.3897 0.042 Uiso 1 1 calc R . . C14 C 0.7196(7) 0.0884(6) 2.3434(7) 0.028(2) Uani 1 1 d . . . H14A H 0.7740 0.0689 2.3606 0.034 Uiso 1 1 calc R . . C15 C 0.7142(7) 0.1553(5) 2.3009(7) 0.026(2) Uani 1 1 d . . . H15A H 0.7666 0.1808 2.2900 0.031 Uiso 1 1 calc R . . C16 C 0.3996(6) 0.1646(5) 2.2950(7) 0.023(2) Uani 1 1 d . . . C17 C 0.3240(7) 0.1586(6) 2.2439(7) 0.029(2) Uani 1 1 d . . . H17A H 0.3271 0.1624 2.1831 0.035 Uiso 1 1 calc R . . C18 C 0.2444(8) 0.1468(7) 2.2846(9) 0.041(3) Uani 1 1 d . . . H18A H 0.1924 0.1435 2.2518 0.050 Uiso 1 1 calc R . . C19 C 0.2422(8) 0.1401(7) 2.3728(9) 0.045(3) Uani 1 1 d . . . H19A H 0.1890 0.1318 2.4017 0.054 Uiso 1 1 calc R . . C20 C 0.3170(8) 0.1455(7) 2.4169(8) 0.041(3) Uani 1 1 d . . . H20A H 0.3139 0.1398 2.4775 0.049 Uiso 1 1 calc R . . C21 C 0.4292(6) 0.1517(5) 1.8995(6) 0.0192(19) Uani 1 1 d . . . C22 C 0.4276(8) 0.0866(6) 1.8493(8) 0.038(3) Uani 1 1 d . . . H22A H 0.4802 0.0628 1.8346 0.046 Uiso 1 1 calc R . . C23 C 0.3479(8) 0.0583(6) 1.8218(9) 0.042(3) Uani 1 1 d . . . H23A H 0.3453 0.0153 1.7880 0.051 Uiso 1 1 calc R . . C24 C 0.2699(8) 0.0961(6) 1.8461(7) 0.034(2) Uani 1 1 d . . . H24A H 0.2142 0.0776 1.8312 0.041 Uiso 1 1 calc R . . C25 C 0.2787(7) 0.1602(6) 1.8919(7) 0.031(2) Uani 1 1 d . . . H25A H 0.2275 0.1863 1.9059 0.037 Uiso 1 1 calc R . . C26 C 0.5924(7) 0.1650(5) 1.8922(7) 0.027(2) Uani 1 1 d . . . C27 C 0.6662(8) 0.1509(7) 1.9435(9) 0.044(3) Uani 1 1 d . . . H27A H 0.6629 0.1498 2.0045 0.053 Uiso 1 1 calc R . . C28 C 0.7458(8) 0.1383(7) 1.9001(9) 0.045(3) Uani 1 1 d . . . H28A H 0.7973 0.1302 1.9323 0.054 Uiso 1 1 calc R . . C29 C 0.7489(8) 0.1379(7) 1.8092(9) 0.046(3) Uani 1 1 d . . . H29A H 0.8010 0.1264 1.7798 0.055 Uiso 1 1 calc R . . C30 C 0.6718(8) 0.1553(8) 1.7630(8) 0.044(3) Uani 1 1 d . . . H30A H 0.6738 0.1576 1.7021 0.053 Uiso 1 1 calc R . . C31 C 0.5090(6) 0.2139(5) 2.0171(7) 0.022(2) Uani 1 1 d . . . C32 C 0.4857(6) 0.2147(5) 2.1728(7) 0.024(2) Uani 1 1 d . . . C33 C 0.4998(7) 0.3300(4) 2.0943(7) 0.0225(18) Uani 1 1 d . . . C34 C 0.4819(7) 0.2927(5) 2.1723(7) 0.023(2) Uani 1 1 d . . . H34A H 0.4426 0.3169 2.2146 0.028 Uiso 1 1 calc R . . C35 C 0.4961(8) 0.1762(4) 2.0929(8) 0.026(2) Uani 1 1 d . . . H35A H 0.4942 0.1245 2.0923 0.032 Uiso 1 1 calc R . . C36 C 0.5160(7) 0.2922(6) 2.0179(8) 0.027(2) Uani 1 1 d . . . H36A H 0.5586 0.3145 1.9773 0.033 Uiso 1 1 calc R . . C37 C 0.5051(10) 0.6427(8) 1.9012(11) 0.065(4) Uani 1 1 d . . . H37A H 0.5537 0.6622 1.9350 0.097 Uiso 1 1 calc R . . H37B H 0.4685 0.6125 1.9382 0.097 Uiso 1 1 calc R . . H37C H 0.4707 0.6830 1.8778 0.097 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 0.0283(4) 0.0358(4) 0.0437(6) 0.0170(4) -0.0045(4) -0.0038(3) Ag2 0.0271(4) 0.0320(3) 0.0361(5) -0.0100(3) -0.0014(3) 0.0025(3) Ag3 0.0420(5) 0.0585(5) 0.0307(5) 0.0064(4) -0.0107(4) -0.0181(4) Ag4 0.0457(6) 0.1486(13) 0.0355(6) 0.0257(7) 0.0017(5) 0.0349(7) N1 0.039(5) 0.024(4) 0.025(5) -0.001(3) 0.003(4) -0.002(3) N2 0.026(4) 0.026(4) 0.018(5) 0.000(3) -0.001(3) 0.007(3) N3 0.025(4) 0.020(3) 0.029(5) 0.004(4) 0.002(3) 0.001(3) N4 0.021(4) 0.021(3) 0.016(5) -0.004(3) 0.000(3) 0.002(3) N5 0.024(5) 0.039(5) 0.029(6) -0.002(4) 0.002(4) -0.013(3) N6 0.028(5) 0.037(5) 0.041(7) -0.007(5) -0.002(4) 0.010(4) N7 0.024(4) 0.029(4) 0.020(5) 0.005(3) -0.004(4) 0.001(3) N8 0.030(5) 0.030(4) 0.019(5) 0.001(3) 0.000(4) -0.002(3) N9 0.032(5) 0.063(6) 0.012(5) -0.004(4) -0.003(4) 0.013(4) N10 0.025(4) 0.041(4) 0.018(5) -0.006(4) -0.001(4) 0.008(4) N11 0.025(5) 0.052(5) 0.023(5) -0.004(4) 0.000(4) -0.002(4) N12 0.049(6) 0.034(4) 0.029(6) -0.005(4) 0.007(5) 0.002(4) N13 0.062(9) 0.084(10) 0.051(9) 0.028(8) -0.041(7) -0.011(8) O1 0.036(5) 0.101(8) 0.047(6) 0.005(5) 0.009(4) 0.011(5) O2 0.047(5) 0.050(5) 0.045(6) -0.014(4) -0.006(4) -0.019(4) O3 0.036(5) 0.076(6) 0.042(6) -0.010(5) -0.003(4) -0.014(4) O4 0.134(11) 0.047(5) 0.055(7) 0.001(5) 0.007(7) 0.020(6) O5 0.143(13) 0.104(10) 0.088(10) 0.032(8) 0.068(10) 0.057(9) O6 0.143(11) 0.039(5) 0.040(6) 0.010(4) 0.025(6) 0.015(5) O7 0.039(5) 0.065(5) 0.027(6) 0.003(4) -0.010(4) 0.006(4) O8 0.036(5) 0.060(6) 0.089(8) 0.008(5) 0.018(5) 0.007(4) O9 0.038(5) 0.091(7) 0.049(6) 0.019(5) -0.014(5) 0.010(5) O10 0.094(9) 0.109(10) 0.052(8) 0.018(7) -0.023(7) -0.063(8) O11 0.050(6) 0.109(9) 0.051(7) 0.020(6) -0.006(5) 0.001(6) O12 0.029(6) 0.28(2) 0.194(19) 0.141(18) 0.034(9) 0.029(10) O13 0.24(2) 0.087(9) 0.072(10) 0.042(8) 0.060(12) 0.071(12) C1 0.035(5) 0.010(4) 0.022(6) -0.001(3) 0.001(4) -0.008(3) C2 0.047(7) 0.029(5) 0.039(7) 0.012(5) 0.006(5) -0.007(5) C3 0.054(7) 0.022(5) 0.048(8) 0.009(5) 0.015(6) -0.003(4) C4 0.038(7) 0.035(6) 0.055(9) 0.007(5) 0.008(6) -0.004(5) C5 0.026(6) 0.046(6) 0.028(7) 0.009(5) -0.002(5) -0.005(4) C6 0.037(6) 0.041(6) 0.019(6) 0.010(5) 0.008(5) 0.000(5) C7 0.044(7) 0.031(5) 0.034(7) -0.003(5) 0.010(5) -0.008(4) C8 0.045(7) 0.045(6) 0.041(8) -0.008(5) 0.007(6) 0.007(5) C9 0.038(7) 0.045(6) 0.047(8) 0.003(6) 0.015(6) 0.014(5) C10 0.040(7) 0.044(6) 0.030(7) 0.011(5) -0.003(5) 0.005(5) C11 0.023(5) 0.023(4) 0.028(6) -0.010(4) 0.001(4) -0.010(3) C12 0.028(5) 0.023(5) 0.040(7) -0.003(4) -0.012(5) -0.008(4) C13 0.043(7) 0.025(5) 0.036(7) 0.008(5) -0.007(5) 0.008(4) C14 0.017(5) 0.038(5) 0.029(6) -0.001(5) -0.008(4) 0.005(4) C15 0.031(5) 0.028(5) 0.018(6) 0.001(4) 0.002(4) -0.001(4) C16 0.026(5) 0.023(5) 0.021(6) 0.014(4) -0.001(4) -0.001(4) C17 0.020(5) 0.047(6) 0.022(6) 0.010(4) -0.002(4) 0.001(4) C18 0.027(6) 0.050(7) 0.047(9) -0.001(6) -0.011(5) -0.004(5) C19 0.022(6) 0.068(8) 0.044(8) 0.003(6) 0.006(5) 0.005(5) C20 0.037(7) 0.060(7) 0.026(7) -0.004(5) 0.016(5) -0.009(5) C21 0.023(5) 0.028(4) 0.007(5) -0.002(4) -0.003(4) 0.000(3) C22 0.040(6) 0.038(6) 0.036(7) -0.012(5) -0.002(5) 0.000(5) C23 0.049(7) 0.029(5) 0.050(8) -0.023(5) -0.008(6) 0.006(5) C24 0.041(6) 0.037(5) 0.024(6) 0.005(5) -0.004(5) -0.006(4) C25 0.025(5) 0.044(6) 0.023(6) -0.004(5) 0.003(4) -0.001(4) C26 0.028(5) 0.030(5) 0.023(6) 0.006(4) -0.002(4) 0.007(4) C27 0.029(6) 0.063(7) 0.042(8) -0.009(6) -0.001(5) -0.009(5) C28 0.029(6) 0.066(8) 0.039(8) -0.007(6) -0.001(5) -0.003(5) C29 0.029(6) 0.060(7) 0.048(9) -0.005(6) 0.003(5) 0.012(5) C30 0.033(6) 0.080(9) 0.019(7) -0.004(6) -0.004(5) 0.015(6) C31 0.024(5) 0.027(4) 0.017(5) -0.007(4) -0.004(4) 0.000(4) C32 0.023(5) 0.022(4) 0.028(6) -0.002(4) 0.001(4) -0.006(4) C33 0.025(4) 0.022(4) 0.020(5) 0.005(4) -0.006(4) -0.002(4) C34 0.019(5) 0.031(5) 0.019(6) 0.000(4) -0.005(4) 0.001(4) C35 0.027(5) 0.024(4) 0.029(6) 0.007(5) -0.006(4) 0.000(4) C36 0.021(5) 0.038(5) 0.023(6) 0.005(5) -0.003(4) -0.001(4) C37 0.063(10) 0.060(8) 0.070(11) -0.019(8) -0.004(8) 0.008(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 N1 2.288(8) . ? Ag1 N4 2.288(8) . ? Ag1 C34 2.649(11) . ? Ag2 N2 2.316(8) . ? Ag2 N8 2.343(8) . ? Ag2 C36 2.635(11) . ? Ag3 N5 2.254(9) . ? Ag3 O2 2.447(10) . ? Ag3 O4 2.451(11) . ? Ag4 N9 2.237(9) . ? Ag4 O7 2.448(10) . ? Ag4 O8 2.540(11) . ? N1 C1 1.332(14) . ? N1 C5 1.353(14) . ? N2 C6 1.340(15) . ? N2 C10 1.349(14) . ? N3 C1 1.403(14) . ? N3 C6 1.404(14) . ? N3 C33 1.438(11) . ? N4 C15 1.330(13) . ? N4 C11 1.357(12) . ? N5 C16 1.333(13) . ? N5 C20 1.368(13) . ? N6 O9 1.223(13) . ? N6 O8 1.244(12) . ? N6 O7 1.270(13) . ? N7 C11 1.397(13) . ? N7 C32 1.415(14) . ? N7 C16 1.420(12) . ? N8 C21 1.308(13) . ? N8 C25 1.350(14) . ? N9 C26 1.345(14) . ? N9 C30 1.356(14) . ? N10 C26 1.400(13) . ? N10 C21 1.408(13) . ? N10 C31 1.441(13) . ? N11 O3 1.214(13) . ? N11 O1 1.225(12) . ? N11 O2 1.260(12) . ? N12 O6 1.210(12) . ? N12 O5 1.215(14) . ? N12 O4 1.242(13) . ? N13 O11 1.190(18) . ? N13 O10 1.23(2) . ? N13 O12 1.252(18) . ? O13 C37 1.329(19) . ? O13 H13 0.8200 . ? C1 C2 1.407(13) . ? C2 C3 1.374(17) . ? C2 H2A 0.9300 . ? C3 C4 1.341(18) . ? C3 H3A 0.9300 . ? C4 C5 1.406(16) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.378(16) . ? C7 C8 1.363(17) . ? C7 H7A 0.9300 . ? C8 C9 1.404(19) . ? C8 H8A 0.9300 . ? C9 C10 1.375(17) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C11 C12 1.396(15) . ? C12 C13 1.378(16) . ? C12 H12A 0.9300 . ? C13 C14 1.359(16) . ? C13 H13A 0.9300 . ? C14 C15 1.368(14) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.382(15) . ? C17 C18 1.371(15) . ? C17 H17A 0.9300 . ? C18 C19 1.349(18) . ? C18 H18A 0.9300 . ? C19 C20 1.314(18) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.398(14) . ? C22 C23 1.369(18) . ? C22 H22A 0.9300 . ? C23 C24 1.410(16) . ? C23 H23A 0.9300 . ? C24 C25 1.355(16) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 C27 1.382(17) . ? C27 C28 1.392(17) . ? C27 H27A 0.9300 . ? C28 C29 1.385(19) . ? C28 H28A 0.9300 . ? C29 C30 1.392(18) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C35 1.354(16) . ? C31 C36 1.412(14) . ? C32 C34 1.403(13) . ? C32 C35 1.410(16) . ? C33 C36 1.370(16) . ? C33 C34 1.393(15) . ? C34 H34A 0.9800 . ? C35 H35A 0.9300 . ? C36 H36A 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N4 173.3(3) . . ? N1 Ag1 C34 86.2(3) . . ? N4 Ag1 C34 87.1(3) . . ? N2 Ag2 N8 167.4(3) . . ? N2 Ag2 C36 86.6(3) . . ? N8 Ag2 C36 85.5(3) . . ? N5 Ag3 O2 142.1(3) . . ? N5 Ag3 O4 104.5(4) . . ? O2 Ag3 O4 111.9(4) . . ? N9 Ag4 O7 140.0(3) . . ? N9 Ag4 O8 158.1(3) . . ? O7 Ag4 O8 51.5(3) . . ? C1 N1 C5 118.7(9) . . ? C1 N1 Ag1 129.1(7) . . ? C5 N1 Ag1 112.0(7) . . ? C6 N2 C10 118.5(10) . . ? C6 N2 Ag2 128.1(7) . . ? C10 N2 Ag2 112.9(8) . . ? C1 N3 C6 124.2(7) . . ? C1 N3 C33 117.9(8) . . ? C6 N3 C33 117.9(9) . . ? C15 N4 C11 118.6(8) . . ? C15 N4 Ag1 114.2(6) . . ? C11 N4 Ag1 127.0(7) . . ? C16 N5 C20 114.2(9) . . ? C16 N5 Ag3 130.2(6) . . ? C20 N5 Ag3 115.6(8) . . ? O9 N6 O8 122.7(11) . . ? O9 N6 O7 117.8(10) . . ? O8 N6 O7 119.3(10) . . ? C11 N7 C32 117.7(8) . . ? C11 N7 C16 122.5(8) . . ? C32 N7 C16 119.4(8) . . ? C21 N8 C25 118.0(9) . . ? C21 N8 Ag2 127.7(7) . . ? C25 N8 Ag2 113.9(7) . . ? C26 N9 C30 118.0(9) . . ? C26 N9 Ag4 122.3(7) . . ? C30 N9 Ag4 117.3(8) . . ? C26 N10 C21 123.7(8) . . ? C26 N10 C31 119.2(9) . . ? C21 N10 C31 116.8(8) . . ? O3 N11 O1 121.8(10) . . ? O3 N11 O2 119.6(9) . . ? O1 N11 O2 118.7(10) . . ? O6 N12 O5 120.2(10) . . ? O6 N12 O4 120.7(10) . . ? O5 N12 O4 119.1(11) . . ? O11 N13 O10 123.6(16) . . ? O11 N13 O12 124(2) . . ? O10 N13 O12 112.2(19) . . ? N11 O2 Ag3 98.8(7) . . ? N12 O4 Ag3 105.8(8) . . ? N6 O7 Ag4 96.4(6) . . ? N6 O8 Ag4 92.7(8) . . ? C37 O13 H13 109.5 . . ? N1 C1 N3 117.3(8) . . ? N1 C1 C2 122.2(10) . . ? N3 C1 C2 120.5(10) . . ? C3 C2 C1 117.5(11) . . ? C3 C2 H2A 121.3 . . ? C1 C2 H2A 121.3 . . ? C4 C3 C2 121.6(10) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 118.4(11) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? N1 C5 C4 121.6(11) . . ? N1 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? N2 C6 C7 122.5(10) . . ? N2 C6 N3 116.9(9) . . ? C7 C6 N3 120.5(11) . . ? C8 C7 C6 119.1(12) . . ? C8 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? C7 C8 C9 119.3(11) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 118.4(11) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? N2 C10 C9 122.1(12) . . ? N2 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? N4 C11 C12 120.2(9) . . ? N4 C11 N7 118.9(9) . . ? C12 C11 N7 121.0(8) . . ? C13 C12 C11 119.0(10) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C14 C13 C12 120.3(10) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C13 C14 C15 118.0(9) . . ? C13 C14 H14A 121.0 . . ? C15 C14 H14A 121.0 . . ? N4 C15 C14 123.8(9) . . ? N4 C15 H15A 118.1 . . ? C14 C15 H15A 118.1 . . ? N5 C16 C17 123.1(9) . . ? N5 C16 N7 117.2(9) . . ? C17 C16 N7 119.7(9) . . ? C18 C17 C16 118.6(10) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? C19 C18 C17 119.3(11) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C20 C19 C18 118.6(11) . . ? C20 C19 H19A 120.7 . . ? C18 C19 H19A 120.7 . . ? C19 C20 N5 126.2(12) . . ? C19 C20 H20A 116.9 . . ? N5 C20 H20A 116.9 . . ? N8 C21 C22 122.3(10) . . ? N8 C21 N10 118.3(8) . . ? C22 C21 N10 119.4(9) . . ? C23 C22 C21 119.5(10) . . ? C23 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C22 C23 C24 118.2(10) . . ? C22 C23 H23A 120.9 . . ? C24 C23 H23A 120.9 . . ? C25 C24 C23 117.7(11) . . ? C25 C24 H24A 121.1 . . ? C23 C24 H24A 121.1 . . ? N8 C25 C24 124.2(10) . . ? N8 C25 H25A 117.9 . . ? C24 C25 H25A 117.9 . . ? N9 C26 C27 123.9(10) . . ? N9 C26 N10 116.7(9) . . ? C27 C26 N10 119.4(10) . . ? C26 C27 C28 117.1(12) . . ? C26 C27 H27A 121.5 . . ? C28 C27 H27A 121.5 . . ? C29 C28 C27 120.7(12) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C28 C29 C30 118.1(11) . . ? C28 C29 H29A 120.9 . . ? C30 C29 H29A 120.9 . . ? N9 C30 C29 122.1(11) . . ? N9 C30 H30A 118.9 . . ? C29 C30 H30A 118.9 . . ? C35 C31 C36 120.2(10) . . ? C35 C31 N10 122.8(9) . . ? C36 C31 N10 116.9(9) . . ? C34 C32 C35 119.5(10) . . ? C34 C32 N7 118.5(9) . . ? C35 C32 N7 121.9(8) . . ? C36 C33 C34 121.4(8) . . ? C36 C33 N3 120.8(10) . . ? C34 C33 N3 117.8(10) . . ? C33 C34 C32 118.5(10) . . ? C33 C34 Ag1 86.8(7) . . ? C32 C34 Ag1 89.4(6) . . ? C33 C34 H34A 117.8 . . ? C32 C34 H34A 117.8 . . ? Ag1 C34 H34A 117.8 . . ? C31 C35 C32 120.4(7) . . ? C31 C35 H35A 119.8 . . ? C32 C35 H35A 119.8 . . ? C33 C36 C31 119.2(10) . . ? C33 C36 Ag2 87.6(7) . . ? C31 C36 Ag2 91.8(6) . . ? C33 C36 H36A 116.9 . . ? C31 C36 H36A 116.9 . . ? Ag2 C36 H36A 116.9 . . ? O13 C37 H37A 109.5 . . ? O13 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O13 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.913 _refine_diff_density_max 3.995 _refine_diff_density_min -2.359 _refine_diff_density_rms 0.145