#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wanzhi Chen' _publ_contact_author_email CHENWZZ@ZJU.EDU.CN _publ_section_title ; Synthesis, Structural Characterization, and Catalytic Behaviour in Heck Coupling of Palladium(II) Complexes Containning Pyrimidine-Functionalized N-Heterocyclic Carbenes ; loop_ _publ_author_name 'Wanzhi Chen.' 'Daqi Wang.' 'Jiansheng Ye.' # Attachment 'w0708.cif' data_w0708 _database_code_depnum_ccdc_archive 'CCDC 675961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 Ag F6 N8 P' _chemical_formula_weight 657.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _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 11.3286(2) _cell_length_b 19.3969(4) _cell_length_c 25.0274(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.8260(10) _cell_angle_gamma 90.00 _cell_volume 5382.78(18) _cell_formula_units_Z 8 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9813 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.20 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 0.878 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8039 _exptl_absorpt_correction_T_max 0.8580 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 30316 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4752 _reflns_number_gt 4298 _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^)+(0.0626P)^2^+12.6231P] 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 4752 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.75688(2) 0.166943(14) 0.473033(10) 0.04706(12) Uani 1 1 d . . . F1 F 0.4456(5) 0.1146(3) 0.7057(2) 0.171(2) Uani 1 1 d . . . F2 F 0.6197(4) 0.1684(3) 0.7284(2) 0.1468(18) Uani 1 1 d . . . F3 F 0.4499(4) 0.2239(3) 0.70755(17) 0.1492(17) Uani 1 1 d . . . F4 F 0.9404(8) 0.0016(5) 0.7101(4) 0.132(6) Uani 0.63(3) 1 d P A 1 F5 F 0.9368(7) 0.1148(5) 0.7083(4) 0.124(6) Uani 0.63(3) 1 d P A 1 F4' F 1.0000 -0.0164(9) 0.7500 0.124(9) Uani 0.37(3) 2 d SP A 2 F4" F 1.0000 0.1477(9) 0.7500 0.116(10) Uani 0.37(3) 2 d SP A 2 F5' F 0.9062(11) 0.0634(11) 0.6967(5) 0.111(9) Uani 0.37(3) 1 d P A 2 F6 F 1.1083(4) 0.0630(2) 0.71958(17) 0.1270(13) Uani 1 1 d . A . N1 N 0.5029(2) 0.20918(14) 0.49547(11) 0.0429(6) Uani 1 1 d . . . N2 N 0.6127(3) 0.16247(15) 0.56536(12) 0.0459(7) Uani 1 1 d . B . N3 N 0.5359(3) 0.24145(17) 0.40960(12) 0.0555(7) Uani 1 1 d . . . N4 N 0.3425(3) 0.24931(19) 0.43125(13) 0.0612(8) Uani 1 1 d . . . N5 N 1.0039(3) 0.11851(17) 0.44585(13) 0.0561(8) Uani 1 1 d . . . N6 N 0.8877(4) 0.16176(18) 0.37593(16) 0.0653(9) Uani 1 1 d . C . N7 N 0.9807(3) 0.09264(19) 0.53446(14) 0.0631(8) Uani 1 1 d . . . N8 N 1.1646(3) 0.0716(2) 0.50619(17) 0.0767(10) Uani 1 1 d . . . P1 P 0.5000 0.16619(10) 0.7500 0.0716(5) Uani 1 2 d S . . P2 P 1.0000 0.06116(11) 0.7500 0.0736(5) Uani 1 2 d S . . C1 C 0.6150(3) 0.18096(17) 0.51417(14) 0.0422(7) Uani 1 1 d . . . C2 C 0.5035(3) 0.1783(2) 0.57928(16) 0.0551(9) Uani 1 1 d . . . H2 H 0.4824 0.1700 0.6127 0.066 Uiso 1 1 calc R . . C3 C 0.4349(3) 0.2076(2) 0.53580(14) 0.0514(8) Uani 1 1 d . . . H3 H 0.3567 0.2240 0.5329 0.062 Uiso 1 1 calc R . . C4 C 0.4581(3) 0.23495(18) 0.44205(14) 0.0445(7) Uani 1 1 d . . . C5 C 0.2990(4) 0.2723(3) 0.38071(18) 0.0692(11) Uani 1 1 d . . . H5 H 0.2173 0.2825 0.3708 0.083 Uiso 1 1 calc R . . C6 C 0.3692(4) 0.2815(2) 0.34302(17) 0.0672(11) Uani 1 1 d . . . H6 H 0.3377 0.2978 0.3081 0.081 Uiso 1 1 calc R . . C7 C 0.4885(4) 0.2653(2) 0.35960(17) 0.0638(10) Uani 1 1 d . . . H7 H 0.5391 0.2711 0.3350 0.077 Uiso 1 1 calc R . . C8 C 0.7092(3) 0.1229(2) 0.60076(15) 0.0528(8) Uani 1 1 d . . . H8A H 0.7043 0.1299 0.6386 0.063 Uiso 0.813(19) 1 calc PR B 1 H8B H 0.7869 0.1398 0.5960 0.063 Uiso 0.813(19) 1 calc PR B 1 H8C H 0.7381 0.1486 0.6341 0.063 Uiso 0.187(19) 1 d PR B 2 H8D H 0.7763 0.1167 0.5826 0.063 Uiso 0.187(19) 1 d PR B 2 C9 C 0.6999(6) 0.0463(3) 0.5878(4) 0.0611(19) Uani 0.813(19) 1 d P B 1 H9A H 0.7122 0.0393 0.5510 0.073 Uiso 0.813(19) 1 calc PR B 1 H9B H 0.7640 0.0223 0.6125 0.073 Uiso 0.813(19) 1 calc PR B 1 C10 C 0.5806(7) 0.0150(3) 0.5925(4) 0.074(2) Uani 0.813(19) 1 d P B 1 H10A H 0.5676 0.0222 0.6293 0.089 Uiso 0.813(19) 1 calc PR B 1 H10B H 0.5163 0.0382 0.5675 0.089 Uiso 0.813(19) 1 calc PR B 1 C9' C 0.666(3) 0.0532(15) 0.6137(18) 0.069(9) Uani 0.187(19) 1 d P B 2 H9'1 H 0.6023 0.0591 0.6338 0.082 Uiso 0.187(19) 1 calc PR B 2 H9'2 H 0.7323 0.0296 0.6375 0.082 Uiso 0.187(19) 1 calc PR B 2 C10' C 0.621(3) 0.0084(13) 0.5653(15) 0.065(9) Uani 0.187(19) 1 d P B 2 H10C H 0.6853 0.0009 0.5458 0.078 Uiso 0.187(19) 1 calc PR B 2 H10D H 0.5560 0.0322 0.5409 0.078 Uiso 0.187(19) 1 calc PR B 2 C11 C 0.5752(6) -0.0602(3) 0.5802(3) 0.1005(18) Uani 1 1 d . . . H11A H 0.4982 -0.0781 0.5838 0.151 Uiso 0.813(19) 1 calc PR B 1 H11B H 0.6379 -0.0835 0.6054 0.151 Uiso 0.813(19) 1 calc PR B 1 H11C H 0.5861 -0.0675 0.5436 0.151 Uiso 0.813(19) 1 calc PR B 1 H11D H 0.6264 -0.0786 0.6124 0.151 Uiso 0.187(19) 1 d PR B 2 H11E H 0.5736 -0.0913 0.5503 0.151 Uiso 0.187(19) 1 d PR B 2 H11F H 0.4950 -0.0545 0.5865 0.151 Uiso 0.187(19) 1 d PR B 2 C12 C 0.8921(3) 0.1467(2) 0.42875(16) 0.0537(9) Uani 1 1 d . . . C13 C 0.9943(4) 0.1433(3) 0.3604(2) 0.0759(12) Uani 1 1 d . . . H13 H 1.0116 0.1488 0.3259 0.091 Uiso 1 1 calc R . . C14 C 1.0658(4) 0.1169(2) 0.40291(19) 0.0709(12) Uani 1 1 d . . . H14 H 1.1433 0.1001 0.4044 0.085 Uiso 1 1 calc R . . C15 C 1.0525(3) 0.0928(2) 0.49896(17) 0.0563(9) Uani 1 1 d . . . C16 C 1.2101(5) 0.0476(3) 0.5552(2) 0.0869(15) Uani 1 1 d . . . H16 H 1.2894 0.0320 0.5624 0.104 Uiso 1 1 calc R . . C17 C 1.1466(5) 0.0445(3) 0.5962(2) 0.0814(13) Uani 1 1 d . . . H17 H 1.1806 0.0275 0.6307 0.098 Uiso 1 1 calc R . . C18 C 1.0298(4) 0.0679(3) 0.5834(2) 0.0719(12) Uani 1 1 d . . . H18 H 0.9834 0.0663 0.6100 0.086 Uiso 1 1 calc R . . C19 C 0.7829(4) 0.1930(3) 0.33980(19) 0.0756(12) Uani 1 1 d . . . H19A H 0.8094 0.2176 0.3106 0.091 Uiso 0.556(13) 1 calc PR C 1 H19B H 0.7456 0.2260 0.3603 0.091 Uiso 0.556(13) 1 calc PR C 1 H19C H 0.8054 0.2397 0.3324 0.091 Uiso 0.444(13) 1 d PR C 2 H19D H 0.7188 0.1964 0.3601 0.091 Uiso 0.444(13) 1 d PR C 2 C20 C 0.6903(10) 0.1389(6) 0.3153(5) 0.084(3) Uani 0.556(13) 1 d P C 1 H20A H 0.6639 0.1158 0.3452 0.101 Uiso 0.556(13) 1 calc PR C 1 H20B H 0.6208 0.1629 0.2944 0.101 Uiso 0.556(13) 1 calc PR C 1 C20' C 0.7340(14) 0.1606(7) 0.2868(7) 0.092(4) Uani 0.444(13) 1 d P C 2 H20C H 0.6535 0.1791 0.2743 0.110 Uiso 0.444(13) 1 calc PR C 2 H20D H 0.7823 0.1771 0.2616 0.110 Uiso 0.444(13) 1 calc PR C 2 C21 C 0.7248(8) 0.0857(4) 0.2801(3) 0.128(3) Uani 1 1 d . . . H21A H 0.6648 0.0493 0.2756 0.154 Uiso 0.556(13) 1 calc PR C 1 H21B H 0.8009 0.0658 0.2985 0.154 Uiso 0.556(13) 1 calc PR C 1 H21C H 0.8042 0.0704 0.2763 0.154 Uiso 0.444(13) 1 d PR C 2 H21D H 0.7124 0.0672 0.3146 0.154 Uiso 0.444(13) 1 d PR C 2 C22 C 0.7377(16) 0.1093(9) 0.2248(6) 0.146(7) Uani 0.556(13) 1 d P C 1 H22A H 0.7466 0.0700 0.2026 0.219 Uiso 0.556(13) 1 calc PR C 1 H22B H 0.8075 0.1383 0.2281 0.219 Uiso 0.556(13) 1 calc PR C 1 H22C H 0.6672 0.1348 0.2080 0.219 Uiso 0.556(13) 1 calc PR C 1 C22' C 0.6324(18) 0.0504(10) 0.2394(8) 0.140(8) Uani 0.444(13) 1 d P C 2 H22D H 0.5881 0.0838 0.2149 0.210 Uiso 0.444(13) 1 calc PR C 2 H22E H 0.5781 0.0261 0.2576 0.210 Uiso 0.444(13) 1 calc PR C 2 H22F H 0.6706 0.0183 0.2191 0.210 Uiso 0.444(13) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.03702(17) 0.05550(19) 0.05251(19) -0.00529(11) 0.01814(12) 0.00102(10) F1 0.209(5) 0.175(5) 0.138(4) -0.071(3) 0.058(4) -0.062(4) F2 0.113(3) 0.205(5) 0.141(4) 0.019(3) 0.068(3) 0.016(3) F3 0.143(4) 0.172(4) 0.117(3) 0.049(3) -0.010(3) 0.006(3) F4 0.142(8) 0.132(9) 0.116(8) -0.041(7) 0.015(6) -0.015(7) F5 0.116(6) 0.125(11) 0.127(10) 0.055(9) 0.014(6) 0.015(7) F4' 0.129(16) 0.123(13) 0.12(2) 0.000 0.029(17) 0.000 F4" 0.137(19) 0.117(11) 0.107(19) 0.000 0.054(16) 0.000 F5' 0.100(7) 0.15(2) 0.080(6) -0.006(8) -0.002(5) 0.010(8) F6 0.113(3) 0.164(4) 0.120(3) -0.003(3) 0.061(2) 0.006(3) N1 0.0335(13) 0.0516(15) 0.0449(14) -0.0027(12) 0.0112(11) 0.0033(11) N2 0.0371(14) 0.0575(17) 0.0439(15) -0.0042(12) 0.0101(12) 0.0033(12) N3 0.0467(16) 0.067(2) 0.0546(18) 0.0081(15) 0.0149(14) 0.0087(14) N4 0.0416(16) 0.083(2) 0.0582(19) 0.0066(17) 0.0087(14) 0.0112(15) N5 0.0489(16) 0.0614(19) 0.0654(19) -0.0063(15) 0.0294(15) 0.0066(14) N6 0.065(2) 0.074(2) 0.065(2) -0.0021(17) 0.0330(18) 0.0090(16) N7 0.0511(18) 0.076(2) 0.066(2) -0.0031(17) 0.0208(16) 0.0070(16) N8 0.058(2) 0.092(3) 0.084(3) 0.000(2) 0.0243(19) 0.0191(19) P1 0.0706(10) 0.1048(14) 0.0414(7) 0.000 0.0161(7) 0.000 P2 0.0718(10) 0.1015(14) 0.0485(8) 0.000 0.0146(7) 0.000 C1 0.0339(15) 0.0466(17) 0.0475(18) -0.0051(14) 0.0116(13) 0.0001(13) C2 0.0443(19) 0.073(2) 0.052(2) -0.0020(17) 0.0194(16) 0.0069(17) C3 0.0379(17) 0.068(2) 0.0514(19) -0.0020(17) 0.0153(15) 0.0089(15) C4 0.0373(16) 0.0492(18) 0.0472(18) -0.0045(14) 0.0090(14) 0.0017(14) C5 0.047(2) 0.092(3) 0.066(3) 0.012(2) 0.0053(18) 0.014(2) C6 0.063(2) 0.079(3) 0.056(2) 0.009(2) 0.0025(19) 0.011(2) C7 0.061(2) 0.077(3) 0.057(2) 0.010(2) 0.0189(18) 0.009(2) C8 0.0404(17) 0.065(2) 0.051(2) 0.0017(17) 0.0056(15) 0.0043(16) C9 0.052(3) 0.065(3) 0.065(4) 0.002(3) 0.010(3) 0.006(3) C10 0.064(4) 0.069(4) 0.088(5) -0.003(3) 0.015(4) 0.001(3) C9' 0.058(16) 0.075(17) 0.07(2) -0.002(14) 0.011(14) 0.002(12) C10' 0.059(15) 0.068(15) 0.068(19) -0.005(13) 0.011(13) 0.003(12) C11 0.095(4) 0.079(4) 0.122(5) -0.010(3) 0.009(3) -0.012(3) C12 0.052(2) 0.055(2) 0.061(2) -0.0059(17) 0.0269(17) 0.0017(17) C13 0.073(3) 0.093(3) 0.073(3) 0.001(3) 0.040(2) 0.010(3) C14 0.062(2) 0.084(3) 0.077(3) -0.003(2) 0.038(2) 0.013(2) C15 0.0493(19) 0.056(2) 0.068(2) -0.0105(18) 0.0237(17) 0.0040(16) C16 0.064(3) 0.102(4) 0.095(4) 0.001(3) 0.017(3) 0.025(3) C17 0.074(3) 0.087(3) 0.081(3) 0.000(3) 0.010(2) 0.019(3) C18 0.063(3) 0.084(3) 0.072(3) -0.002(2) 0.021(2) 0.008(2) C19 0.076(3) 0.085(3) 0.069(3) 0.004(2) 0.023(2) 0.014(3) C20 0.081(6) 0.097(7) 0.074(6) 0.001(5) 0.015(5) 0.017(5) C20' 0.093(10) 0.095(10) 0.086(10) 0.000(7) 0.017(8) 0.010(7) C21 0.131(6) 0.124(6) 0.118(6) 0.000(5) -0.004(5) 0.017(5) C22 0.155(14) 0.150(14) 0.128(12) 0.007(10) 0.019(10) 0.036(11) C22' 0.144(16) 0.132(15) 0.128(14) -0.027(12) -0.006(12) 0.002(12) _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 C1 2.097(3) . ? Ag1 C12 2.104(4) . ? F1 P1 1.525(4) . ? F2 P1 1.560(4) . ? F3 P1 1.567(4) . ? F4 P2 1.586(7) . ? F5 P2 1.542(6) . ? F4' P2 1.504(18) . ? F4" P2 1.679(17) . ? F5' P2 1.527(10) . ? F6 P2 1.571(3) . ? N1 C1 1.374(4) . ? N1 C3 1.389(4) . ? N1 C4 1.420(4) . ? N2 C1 1.336(5) . ? N2 C2 1.386(5) . ? N2 C8 1.474(4) . ? N3 C4 1.321(4) . ? N3 C7 1.339(5) . ? N4 C4 1.312(4) . ? N4 C5 1.336(5) . ? N5 C12 1.365(5) . ? N5 C14 1.399(5) . ? N5 C15 1.421(5) . ? N6 C12 1.345(5) . ? N6 C13 1.390(6) . ? N6 C19 1.468(6) . ? N7 C15 1.322(5) . ? N7 C18 1.327(6) . ? N8 C15 1.312(5) . ? N8 C16 1.315(7) . ? P1 F1 1.525(4) 2_656 ? P1 F2 1.560(4) 2_656 ? P1 F3 1.567(4) 2_656 ? P2 F5' 1.527(10) 2_756 ? P2 F5 1.542(6) 2_756 ? P2 F6 1.571(4) 2_756 ? P2 F4 1.586(7) 2_756 ? C2 C3 1.328(5) . ? C5 C6 1.364(6) . ? C6 C7 1.366(6) . ? C8 C9' 1.49(3) . ? C8 C9 1.519(7) . ? C9 C10 1.509(14) . ? C10 C11 1.489(9) . ? C9' C10' 1.49(6) . ? C10' C11 1.50(3) . ? C13 C14 1.303(7) . ? C16 C17 1.369(8) . ? C17 C18 1.373(6) . ? C19 C20' 1.469(15) . ? C19 C20 1.521(12) . ? C20 C21 1.461(13) . ? C20' C21 1.465(15) . ? C21 C22' 1.471(18) . ? C21 C22 1.495(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ag1 C12 175.77(13) . . ? C1 N1 C3 110.8(3) . . ? C1 N1 C4 126.0(3) . . ? C3 N1 C4 123.2(3) . . ? C1 N2 C2 112.0(3) . . ? C1 N2 C8 123.9(3) . . ? C2 N2 C8 123.7(3) . . ? C4 N3 C7 114.7(3) . . ? C4 N4 C5 115.1(3) . . ? C12 N5 C14 110.3(3) . . ? C12 N5 C15 126.2(3) . . ? C14 N5 C15 123.4(3) . . ? C12 N6 C13 111.1(4) . . ? C12 N6 C19 123.9(4) . . ? C13 N6 C19 125.0(4) . . ? C15 N7 C18 115.0(4) . . ? C15 N8 C16 115.0(4) . . ? F1 P1 F1 98.1(5) . 2_656 ? F1 P1 F2 91.1(3) . 2_656 ? F1 P1 F2 91.0(3) 2_656 2_656 ? F1 P1 F2 91.0(3) . . ? F1 P1 F2 91.1(3) 2_656 . ? F2 P1 F2 176.9(4) 2_656 . ? F1 P1 F3 175.3(3) . 2_656 ? F1 P1 F3 86.5(3) 2_656 2_656 ? F2 P1 F3 88.0(3) 2_656 2_656 ? F2 P1 F3 89.8(3) . 2_656 ? F1 P1 F3 86.5(3) . . ? F1 P1 F3 175.3(3) 2_656 . ? F2 P1 F3 89.8(3) 2_656 . ? F2 P1 F3 88.0(3) . . ? F3 P1 F3 88.9(4) 2_656 . ? F4' P2 F5' 91.7(8) . 2_756 ? F4' P2 F5' 91.7(8) . . ? F5' P2 F5' 176.7(16) 2_756 . ? F4' P2 F5 132.5(5) . 2_756 ? F5' P2 F5 41.1(6) 2_756 2_756 ? F5' P2 F5 135.6(11) . 2_756 ? F4' P2 F5 132.5(5) . . ? F5' P2 F5 135.6(11) 2_756 . ? F5' P2 F5 41.1(6) . . ? F5 P2 F5 95.0(9) 2_756 . ? F4' P2 F6 91.30(19) . 2_756 ? F5' P2 F6 92.8(6) 2_756 2_756 ? F5' P2 F6 87.2(6) . 2_756 ? F5 P2 F6 87.5(3) 2_756 2_756 ? F5 P2 F6 90.7(3) . 2_756 ? F4' P2 F6 91.30(19) . . ? F5' P2 F6 87.2(6) 2_756 . ? F5' P2 F6 92.8(6) . . ? F5 P2 F6 90.7(3) 2_756 . ? F5 P2 F6 87.5(3) . . ? F6 P2 F6 177.4(4) 2_756 . ? F4' P2 F4 43.2(4) . . ? F5' P2 F4 134.6(11) 2_756 . ? F5' P2 F4 48.7(6) . . ? F5 P2 F4 175.7(7) 2_756 . ? F5 P2 F4 89.3(5) . . ? F6 P2 F4 92.7(4) 2_756 . ? F6 P2 F4 89.2(3) . . ? F4' P2 F4 43.2(4) . 2_756 ? F5' P2 F4 48.7(6) 2_756 2_756 ? F5' P2 F4 134.6(11) . 2_756 ? F5 P2 F4 89.3(5) 2_756 2_756 ? F5 P2 F4 175.7(7) . 2_756 ? F6 P2 F4 89.2(3) 2_756 2_756 ? F6 P2 F4 92.7(4) . 2_756 ? F4 P2 F4 86.4(8) . 2_756 ? F4' P2 F4" 180.000(6) . . ? F5' P2 F4" 88.3(8) 2_756 . ? F5' P2 F4" 88.3(8) . . ? F5 P2 F4" 47.5(5) 2_756 . ? F5 P2 F4" 47.5(5) . . ? F6 P2 F4" 88.70(19) 2_756 . ? F6 P2 F4" 88.70(19) . . ? F4 P2 F4" 136.8(4) . . ? F4 P2 F4" 136.8(4) 2_756 . ? N2 C1 N1 103.6(3) . . ? N2 C1 Ag1 127.1(2) . . ? N1 C1 Ag1 129.3(2) . . ? C3 C2 N2 106.9(3) . . ? C2 C3 N1 106.6(3) . . ? N4 C4 N3 128.1(3) . . ? N4 C4 N1 114.7(3) . . ? N3 C4 N1 117.3(3) . . ? N4 C5 C6 123.0(4) . . ? C5 C6 C7 116.1(4) . . ? N3 C7 C6 123.1(4) . . ? N2 C8 C9' 111.6(11) . . ? N2 C8 C9 111.8(3) . . ? C9' C8 C9 31.9(16) . . ? C10 C9 C8 113.6(8) . . ? C11 C10 C9 112.2(8) . . ? C8 C9' C10' 115(4) . . ? C9' C10' C11 113(3) . . ? C10 C11 C10' 35.1(13) . . ? N6 C12 N5 103.9(3) . . ? N6 C12 Ag1 126.3(3) . . ? N5 C12 Ag1 129.7(3) . . ? C14 C13 N6 107.7(4) . . ? C13 C14 N5 107.0(4) . . ? N8 C15 N7 128.2(4) . . ? N8 C15 N5 114.7(4) . . ? N7 C15 N5 117.1(3) . . ? N8 C16 C17 123.3(4) . . ? C16 C17 C18 116.1(5) . . ? N7 C18 C17 122.4(4) . . ? N6 C19 C20' 119.2(6) . . ? N6 C19 C20 111.5(5) . . ? C20' C19 C20 40.6(7) . . ? C21 C20 C19 118.9(9) . . ? C21 C20' C19 122.1(12) . . ? C20 C21 C20' 41.5(7) . . ? C20 C21 C22' 120.4(11) . . ? C20' C21 C22' 124.4(11) . . ? C20 C21 C22 115.5(10) . . ? C20' C21 C22 77.5(11) . . ? C22' C21 C22 72.0(11) . . ? 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 C2 N2 C1 N1 -0.2(4) . . . . ? C8 N2 C1 N1 173.3(3) . . . . ? C2 N2 C1 Ag1 -178.9(3) . . . . ? C8 N2 C1 Ag1 -5.3(5) . . . . ? C3 N1 C1 N2 0.4(4) . . . . ? C4 N1 C1 N2 -177.8(3) . . . . ? C3 N1 C1 Ag1 179.0(3) . . . . ? C4 N1 C1 Ag1 0.8(5) . . . . ? C12 Ag1 C1 N2 102.3(19) . . . . ? C12 Ag1 C1 N1 -76(2) . . . . ? C1 N2 C2 C3 0.0(4) . . . . ? C8 N2 C2 C3 -173.5(3) . . . . ? N2 C2 C3 N1 0.2(4) . . . . ? C1 N1 C3 C2 -0.4(4) . . . . ? C4 N1 C3 C2 177.9(3) . . . . ? C5 N4 C4 N3 1.1(6) . . . . ? C5 N4 C4 N1 -178.7(4) . . . . ? C7 N3 C4 N4 -0.5(6) . . . . ? C7 N3 C4 N1 179.3(3) . . . . ? C1 N1 C4 N4 169.8(3) . . . . ? C3 N1 C4 N4 -8.2(5) . . . . ? C1 N1 C4 N3 -10.1(5) . . . . ? C3 N1 C4 N3 171.9(3) . . . . ? C4 N4 C5 C6 -1.1(7) . . . . ? N4 C5 C6 C7 0.5(7) . . . . ? C4 N3 C7 C6 -0.2(6) . . . . ? C5 C6 C7 N3 0.2(7) . . . . ? C1 N2 C8 C9' -114(2) . . . . ? C2 N2 C8 C9' 59(2) . . . . ? C1 N2 C8 C9 -79.9(6) . . . . ? C2 N2 C8 C9 92.9(6) . . . . ? N2 C8 C9 C10 -57.4(9) . . . . ? C9' C8 C9 C10 39(2) . . . . ? C8 C9 C10 C11 -179.3(5) . . . . ? N2 C8 C9' C10' 59(4) . . . . ? C9 C8 C9' C10' -38(3) . . . . ? C8 C9' C10' C11 -178.3(17) . . . . ? C9 C10 C11 C10' -36.8(18) . . . . ? C9' C10' C11 C10 39(3) . . . . ? C13 N6 C12 N5 0.0(5) . . . . ? C19 N6 C12 N5 179.5(4) . . . . ? C13 N6 C12 Ag1 177.9(3) . . . . ? C19 N6 C12 Ag1 -2.6(6) . . . . ? C14 N5 C12 N6 0.0(5) . . . . ? C15 N5 C12 N6 -178.9(4) . . . . ? C14 N5 C12 Ag1 -177.8(3) . . . . ? C15 N5 C12 Ag1 3.3(6) . . . . ? C1 Ag1 C12 N6 76(2) . . . . ? C1 Ag1 C12 N5 -106.9(19) . . . . ? C12 N6 C13 C14 -0.1(6) . . . . ? C19 N6 C13 C14 -179.5(5) . . . . ? N6 C13 C14 N5 0.0(6) . . . . ? C12 N5 C14 C13 0.0(5) . . . . ? C15 N5 C14 C13 178.9(4) . . . . ? C16 N8 C15 N7 -0.4(7) . . . . ? C16 N8 C15 N5 -179.8(4) . . . . ? C18 N7 C15 N8 0.2(7) . . . . ? C18 N7 C15 N5 179.6(4) . . . . ? C12 N5 C15 N8 -176.5(4) . . . . ? C14 N5 C15 N8 4.7(6) . . . . ? C12 N5 C15 N7 4.0(6) . . . . ? C14 N5 C15 N7 -174.8(4) . . . . ? C15 N8 C16 C17 0.1(8) . . . . ? N8 C16 C17 C18 0.3(9) . . . . ? C15 N7 C18 C17 0.3(7) . . . . ? C16 C17 C18 N7 -0.5(8) . . . . ? C12 N6 C19 C20' -128.8(9) . . . . ? C13 N6 C19 C20' 50.6(11) . . . . ? C12 N6 C19 C20 -84.5(7) . . . . ? C13 N6 C19 C20 94.9(7) . . . . ? N6 C19 C20 C21 -62.1(11) . . . . ? C20' C19 C20 C21 48.0(11) . . . . ? N6 C19 C20' C21 39.7(18) . . . . ? C20 C19 C20' C21 -50.0(13) . . . . ? C19 C20 C21 C20' -46.9(12) . . . . ? C19 C20 C21 C22' -155.9(13) . . . . ? C19 C20 C21 C22 -72.6(13) . . . . ? C19 C20' C21 C20 51.4(13) . . . . ? C19 C20' C21 C22' 150.2(15) . . . . ? C19 C20' C21 C22 -152.2(16) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.705 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.081 #===END data_070713d _database_code_depnum_ccdc_archive 'CCDC 675962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H25 Ag2 F12 N11 P2' _chemical_formula_weight 1021.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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' _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 14.645(2) _cell_length_b 18.615(2) _cell_length_c 15.0318(19) _cell_angle_alpha 90.00 _cell_angle_beta 112.860(2) _cell_angle_gamma 90.00 _cell_volume 3776.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7838 _exptl_absorpt_correction_T_max 0.8675 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 18562 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6660 _reflns_number_gt 4506 _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^)+(0.0486P)^2^+10.1248P] 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 6660 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.029 _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 0.97195(4) 0.12734(2) 0.25575(4) 0.04899(16) Uani 1 1 d . . . Ag2 Ag 0.85760(4) 0.01769(3) 0.09245(4) 0.05530(17) Uani 1 1 d . . . F1 F 0.6001(5) 0.9692(3) 0.7454(7) 0.196(4) Uani 1 1 d . . . F2 F 0.4693(5) 0.8409(4) 0.6389(5) 0.146(2) Uani 1 1 d . . . F3 F 0.5460(9) 0.8734(4) 0.7873(5) 0.215(5) Uani 1 1 d . . . F4 F 0.4458(4) 0.9534(4) 0.6810(5) 0.155(3) Uani 1 1 d . . . F5 F 0.5225(6) 0.9352(4) 0.5900(5) 0.163(3) Uani 1 1 d . . . F6 F 0.6251(5) 0.8605(4) 0.6946(7) 0.173(3) Uani 1 1 d . . . F7 F 0.7478(9) 0.3096(4) 0.0794(10) 0.251(6) Uani 1 1 d . . . F8 F 0.6345(6) 0.1770(4) 0.0747(12) 0.304(8) Uani 1 1 d . . . F9 F 0.7853(4) 0.2043(4) 0.1436(6) 0.163(3) Uani 1 1 d . . . F10 F 0.7191(9) 0.2151(8) -0.0078(6) 0.319(9) Uani 1 1 d . . . F11 F 0.5968(7) 0.2774(6) 0.0000(6) 0.232(5) Uani 1 1 d . . . F12 F 0.6637(7) 0.2745(5) 0.1531(5) 0.179(3) Uani 1 1 d . . . N1 N 0.9899(4) -0.0094(2) 0.3740(3) 0.0440(12) Uani 1 1 d . . . N2 N 0.8346(4) 0.0107(3) 0.2992(3) 0.0451(12) Uani 1 1 d . . . N3 N 1.1277(4) 0.0539(3) 0.3763(4) 0.0596(14) Uani 1 1 d . . . N4 N 1.1461(4) -0.0569(3) 0.4612(4) 0.0644(15) Uani 1 1 d . . . N5 N 0.7151(4) -0.0182(3) 0.0844(4) 0.0488(12) Uani 1 1 d . . . N6 N 1.0791(4) 0.0058(3) 0.1387(4) 0.0477(12) Uani 1 1 d . . . N7 N 1.0328(4) 0.1097(3) 0.0763(4) 0.0495(13) Uani 1 1 d . . . N8 N 0.9928(5) -0.0879(3) 0.1744(5) 0.0672(16) Uani 1 1 d . . . N9 N 1.1648(5) -0.0963(4) 0.2146(6) 0.091(2) Uani 1 1 d . . . N10 N 1.0153(4) 0.2251(3) 0.2014(4) 0.0499(12) Uani 1 1 d . . . N11 N 0.2681(8) 0.7346(5) 0.4952(8) 0.138(4) Uani 1 1 d . . . P1 P 0.53641(14) 0.90499(11) 0.69168(15) 0.0638(5) Uani 1 1 d . . . P2 P 0.69101(17) 0.24148(12) 0.07142(18) 0.0826(7) Uani 1 1 d . . . C1 C 0.9236(4) 0.0387(3) 0.3131(4) 0.0413(13) Uani 1 1 d . . . C2 C 0.8456(5) -0.0539(3) 0.3509(5) 0.0571(17) Uani 1 1 d . . . H2 H 0.7945 -0.0829 0.3526 0.068 Uiso 1 1 calc R . . C3 C 0.9411(5) -0.0661(3) 0.3965(5) 0.0568(17) Uani 1 1 d . . . H3 H 0.9702 -0.1051 0.4360 0.068 Uiso 1 1 calc R . . C4 C 1.0944(5) -0.0027(3) 0.4065(4) 0.0469(15) Uani 1 1 d . . . C5 C 1.2447(6) -0.0507(4) 0.4898(6) 0.078(2) Uani 1 1 d . . . H5 H 1.2850 -0.0870 0.5274 0.093 Uiso 1 1 calc R . . C6 C 1.2880(6) 0.0071(5) 0.4655(6) 0.075(2) Uani 1 1 d . . . H6 H 1.3566 0.0111 0.4870 0.090 Uiso 1 1 calc R . . C7 C 1.2271(5) 0.0588(4) 0.4085(6) 0.073(2) Uani 1 1 d . . . H7 H 1.2550 0.0986 0.3914 0.088 Uiso 1 1 calc R . . C8 C 0.7402(4) 0.0421(3) 0.2365(5) 0.0505(15) Uani 1 1 d . . . H8A H 0.7525 0.0870 0.2102 0.061 Uiso 1 1 calc R . . H8B H 0.7013 0.0528 0.2745 0.061 Uiso 1 1 calc R . . C9 C 0.6814(4) -0.0071(3) 0.1544(4) 0.0461(14) Uani 1 1 d . . . C10 C 0.5944(5) -0.0388(4) 0.1503(5) 0.0625(19) Uani 1 1 d . . . H10 H 0.5715 -0.0302 0.1989 0.075 Uiso 1 1 calc R . . C11 C 0.5417(5) -0.0832(4) 0.0741(6) 0.072(2) Uani 1 1 d . . . H11 H 0.4837 -0.1052 0.0715 0.087 Uiso 1 1 calc R . . C12 C 0.5758(5) -0.0943(4) 0.0025(5) 0.067(2) Uani 1 1 d . . . H12 H 0.5411 -0.1235 -0.0500 0.081 Uiso 1 1 calc R . . C13 C 0.6615(5) -0.0618(4) 0.0097(5) 0.0594(18) Uani 1 1 d . . . H13 H 0.6846 -0.0697 -0.0389 0.071 Uiso 1 1 calc R . . C14 C 0.9980(4) 0.0490(3) 0.0995(4) 0.0422(14) Uani 1 1 d . . . C15 C 1.1343(5) 0.1055(4) 0.1022(5) 0.0617(19) Uani 1 1 d . . . H15 H 1.1746 0.1411 0.0937 0.074 Uiso 1 1 calc R . . C16 C 1.1638(5) 0.0408(4) 0.1418(5) 0.0607(18) Uani 1 1 d . . . H16 H 1.2281 0.0229 0.1664 0.073 Uiso 1 1 calc R . . C17 C 1.0786(5) -0.0640(3) 0.1780(5) 0.0550(17) Uani 1 1 d . . . C18 C 1.1627(9) -0.1608(6) 0.2536(8) 0.116(4) Uani 1 1 d . . . H18 H 1.2219 -0.1862 0.2804 0.139 Uiso 1 1 calc R . . C19 C 1.0808(10) -0.1911(5) 0.2564(7) 0.104(3) Uani 1 1 d . . . H19 H 1.0825 -0.2355 0.2851 0.125 Uiso 1 1 calc R . . C20 C 0.9946(8) -0.1530(4) 0.2147(6) 0.084(2) Uani 1 1 d . . . H20 H 0.9359 -0.1724 0.2141 0.101 Uiso 1 1 calc R . . C21 C 0.9740(6) 0.1742(4) 0.0408(5) 0.0633(19) Uani 1 1 d . . . H21A H 0.9052 0.1634 0.0277 0.076 Uiso 1 1 calc R . . H21B H 0.9783 0.1883 -0.0196 0.076 Uiso 1 1 calc R . . C22 C 1.0063(5) 0.2363(3) 0.1102(5) 0.0506(15) Uani 1 1 d . . . C23 C 1.0255(6) 0.3024(4) 0.0812(6) 0.076(2) Uani 1 1 d . . . H23 H 1.0194 0.3093 0.0178 0.091 Uiso 1 1 calc R . . C24 C 1.0539(7) 0.3587(4) 0.1455(7) 0.088(3) Uani 1 1 d . . . H24 H 1.0655 0.4039 0.1256 0.106 Uiso 1 1 calc R . . C25 C 1.0651(7) 0.3474(4) 0.2395(7) 0.090(3) Uani 1 1 d . . . H25 H 1.0853 0.3843 0.2848 0.108 Uiso 1 1 calc R . . C26 C 1.0451(6) 0.2793(4) 0.2648(6) 0.070(2) Uani 1 1 d . . . H26 H 1.0528 0.2709 0.3284 0.084 Uiso 1 1 calc R . . C27 C 0.2327(9) 0.7530(5) 0.5427(8) 0.101(3) Uani 1 1 d . . . C28 C 0.1837(12) 0.7771(6) 0.6060(10) 0.167(6) Uani 1 1 d . . . H28A H 0.1520 0.8225 0.5836 0.250 Uiso 1 1 calc R . . H28B H 0.2321 0.7823 0.6707 0.250 Uiso 1 1 calc R . . H28C H 0.1350 0.7423 0.6053 0.250 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 0.0601(3) 0.0439(3) 0.0461(3) 0.0056(2) 0.0240(2) -0.0048(2) Ag2 0.0450(3) 0.0665(3) 0.0601(3) -0.0104(3) 0.0267(3) -0.0103(2) F1 0.107(5) 0.075(4) 0.287(10) -0.012(5) -0.054(5) -0.013(3) F2 0.158(6) 0.141(5) 0.131(5) -0.048(4) 0.046(5) -0.066(5) F3 0.440(15) 0.144(6) 0.066(4) -0.006(4) 0.106(6) -0.039(7) F4 0.090(4) 0.219(7) 0.150(6) -0.054(5) 0.041(4) 0.047(4) F5 0.259(9) 0.136(5) 0.146(6) 0.045(5) 0.136(7) 0.052(6) F6 0.112(5) 0.131(5) 0.285(11) 0.024(6) 0.087(6) 0.049(4) F7 0.286(13) 0.113(6) 0.423(18) 0.042(8) 0.212(13) -0.014(7) F8 0.100(5) 0.112(6) 0.61(2) -0.053(9) 0.039(9) -0.037(5) F9 0.081(4) 0.153(6) 0.202(8) 0.066(5) -0.005(4) 0.015(4) F10 0.316(13) 0.50(2) 0.126(7) -0.028(9) 0.064(8) 0.283(14) F11 0.200(8) 0.336(12) 0.120(6) 0.038(7) 0.017(5) 0.192(9) F12 0.239(9) 0.194(7) 0.120(6) 0.022(5) 0.086(6) 0.061(7) N1 0.051(3) 0.043(3) 0.034(3) 0.004(2) 0.012(2) -0.004(2) N2 0.049(3) 0.050(3) 0.039(3) -0.006(2) 0.020(2) -0.009(2) N3 0.053(3) 0.065(4) 0.056(4) 0.015(3) 0.016(3) -0.006(3) N4 0.062(4) 0.063(4) 0.057(4) 0.011(3) 0.012(3) 0.001(3) N5 0.039(3) 0.060(3) 0.047(3) -0.006(3) 0.017(2) -0.005(2) N6 0.044(3) 0.053(3) 0.049(3) -0.012(2) 0.021(3) -0.004(2) N7 0.058(3) 0.050(3) 0.050(3) -0.008(2) 0.030(3) -0.009(3) N8 0.077(4) 0.051(3) 0.082(5) -0.005(3) 0.039(4) -0.009(3) N9 0.068(5) 0.068(4) 0.117(6) 0.006(4) 0.015(4) 0.017(4) N10 0.062(3) 0.042(3) 0.051(3) 0.001(2) 0.027(3) -0.006(2) N11 0.155(9) 0.120(8) 0.164(11) -0.045(7) 0.089(8) -0.011(6) P1 0.0555(11) 0.0706(12) 0.0658(13) -0.0066(10) 0.0241(10) -0.0023(10) P2 0.0757(15) 0.0644(13) 0.0872(17) -0.0011(12) 0.0093(12) 0.0144(12) C1 0.050(4) 0.040(3) 0.035(3) -0.007(3) 0.018(3) -0.006(3) C2 0.064(5) 0.054(4) 0.058(4) 0.005(3) 0.029(4) -0.017(3) C3 0.065(5) 0.051(4) 0.049(4) 0.010(3) 0.016(3) -0.009(3) C4 0.049(4) 0.059(4) 0.030(3) 0.003(3) 0.012(3) -0.009(3) C5 0.071(6) 0.077(5) 0.074(6) 0.014(4) 0.016(4) 0.012(4) C6 0.052(4) 0.094(6) 0.072(5) 0.009(5) 0.017(4) 0.003(4) C7 0.053(5) 0.089(6) 0.075(5) 0.014(5) 0.023(4) -0.009(4) C8 0.047(4) 0.057(4) 0.047(4) -0.012(3) 0.018(3) -0.003(3) C9 0.040(3) 0.053(4) 0.045(4) -0.002(3) 0.017(3) 0.001(3) C10 0.056(4) 0.080(5) 0.062(5) -0.014(4) 0.034(4) -0.016(4) C11 0.052(4) 0.096(6) 0.072(5) -0.017(4) 0.028(4) -0.026(4) C12 0.059(4) 0.081(5) 0.063(5) -0.023(4) 0.026(4) -0.021(4) C13 0.054(4) 0.078(5) 0.054(4) -0.014(4) 0.028(3) -0.007(4) C14 0.040(3) 0.051(3) 0.035(3) -0.008(3) 0.014(3) -0.007(3) C15 0.057(4) 0.066(5) 0.077(5) -0.015(4) 0.043(4) -0.020(4) C16 0.044(4) 0.069(5) 0.078(5) -0.018(4) 0.033(4) -0.009(3) C17 0.064(4) 0.051(4) 0.049(4) -0.017(3) 0.020(3) -0.005(3) C18 0.107(8) 0.073(6) 0.135(10) 0.018(6) 0.013(7) 0.033(6) C19 0.143(10) 0.061(6) 0.088(7) 0.004(5) 0.022(7) -0.013(7) C20 0.115(7) 0.058(5) 0.081(6) -0.008(4) 0.041(6) -0.020(5) C21 0.086(5) 0.063(4) 0.043(4) 0.007(3) 0.028(4) -0.003(4) C22 0.062(4) 0.042(3) 0.048(4) 0.009(3) 0.022(3) 0.003(3) C23 0.105(6) 0.065(5) 0.069(5) 0.015(4) 0.046(5) -0.004(4) C24 0.136(8) 0.043(4) 0.114(8) 0.005(4) 0.079(7) -0.009(5) C25 0.139(8) 0.052(4) 0.103(7) -0.016(4) 0.076(7) -0.023(5) C26 0.105(6) 0.057(4) 0.061(5) -0.010(4) 0.046(5) -0.017(4) C27 0.132(9) 0.072(6) 0.102(8) -0.020(5) 0.049(7) -0.008(6) C28 0.283(18) 0.114(9) 0.160(13) -0.009(9) 0.147(14) 0.018(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C1 2.108(6) . ? Ag1 N10 2.187(5) . ? Ag1 Ag2 3.1308(7) . ? Ag2 C14 2.100(6) . ? Ag2 N5 2.149(5) . ? F1 P1 1.538(6) . ? F2 P1 1.553(6) . ? F3 P1 1.509(6) . ? F4 P1 1.560(6) . ? F5 P1 1.566(6) . ? F6 P1 1.526(6) . ? F7 P2 1.495(8) . ? F8 P2 1.469(9) . ? F9 P2 1.548(6) . ? F10 P2 1.487(8) . ? F11 P2 1.534(7) . ? F12 P2 1.557(7) . ? N1 C1 1.376(7) . ? N1 C3 1.387(7) . ? N1 C4 1.419(8) . ? N2 C1 1.341(7) . ? N2 C2 1.408(8) . ? N2 C8 1.460(8) . ? N3 C4 1.313(8) . ? N3 C7 1.347(8) . ? N4 C4 1.336(8) . ? N4 C5 1.342(9) . ? N5 C9 1.342(7) . ? N5 C13 1.359(8) . ? N6 C14 1.364(8) . ? N6 C16 1.385(8) . ? N6 C17 1.429(8) . ? N7 C14 1.340(7) . ? N7 C15 1.385(8) . ? N7 C21 1.452(8) . ? N8 C17 1.314(8) . ? N8 C20 1.351(10) . ? N9 C17 1.311(9) . ? N9 C18 1.342(12) . ? N10 C26 1.340(8) . ? N10 C22 1.342(8) . ? N11 C27 1.088(11) . ? C2 C3 1.317(9) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C5 C6 1.370(11) . ? C5 H5 0.9300 . ? C6 C7 1.364(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.509(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.383(8) . ? C10 C11 1.379(10) . ? C10 H10 0.9300 . ? C11 C12 1.368(9) . ? C11 H11 0.9300 . ? C12 C13 1.358(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 C16 1.339(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 C19 1.340(14) . ? C18 H18 0.9300 . ? C19 C20 1.369(13) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.504(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.371(9) . ? C23 C24 1.376(11) . ? C23 H23 0.9300 . ? C24 C25 1.374(12) . ? C24 H24 0.9300 . ? C25 C26 1.387(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.467(15) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 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 C1 Ag1 N10 175.2(2) . . ? C1 Ag1 Ag2 69.38(15) . . ? N10 Ag1 Ag2 113.20(14) . . ? C14 Ag2 N5 178.0(2) . . ? C14 Ag2 Ag1 64.16(15) . . ? N5 Ag2 Ag1 117.33(14) . . ? C1 N1 C3 111.0(5) . . ? C1 N1 C4 124.0(5) . . ? C3 N1 C4 124.9(5) . . ? C1 N2 C2 110.5(5) . . ? C1 N2 C8 124.4(5) . . ? C2 N2 C8 125.1(5) . . ? C4 N3 C7 115.2(6) . . ? C4 N4 C5 114.4(6) . . ? C9 N5 C13 118.0(5) . . ? C9 N5 Ag2 123.6(4) . . ? C13 N5 Ag2 118.0(4) . . ? C14 N6 C16 110.8(5) . . ? C14 N6 C17 124.8(5) . . ? C16 N6 C17 124.2(6) . . ? C14 N7 C15 110.7(5) . . ? C14 N7 C21 124.2(5) . . ? C15 N7 C21 124.7(6) . . ? C17 N8 C20 115.6(7) . . ? C17 N9 C18 114.3(8) . . ? C26 N10 C22 119.0(5) . . ? C26 N10 Ag1 115.0(4) . . ? C22 N10 Ag1 125.7(4) . . ? F3 P1 F6 89.9(6) . . ? F3 P1 F1 89.5(5) . . ? F6 P1 F1 94.1(4) . . ? F3 P1 F2 89.6(4) . . ? F6 P1 F2 87.8(4) . . ? F1 P1 F2 178.0(5) . . ? F3 P1 F4 94.8(5) . . ? F6 P1 F4 175.3(5) . . ? F1 P1 F4 85.6(4) . . ? F2 P1 F4 92.7(4) . . ? F3 P1 F5 177.3(5) . . ? F6 P1 F5 90.5(4) . . ? F1 P1 F5 93.2(5) . . ? F2 P1 F5 87.7(4) . . ? F4 P1 F5 84.8(4) . . ? F8 P2 F10 95.2(9) . . ? F8 P2 F7 173.1(8) . . ? F10 P2 F7 91.5(8) . . ? F8 P2 F11 90.8(6) . . ? F10 P2 F11 92.2(5) . . ? F7 P2 F11 90.4(6) . . ? F8 P2 F9 88.4(5) . . ? F10 P2 F9 88.0(5) . . ? F7 P2 F9 90.3(5) . . ? F11 P2 F9 179.2(6) . . ? F8 P2 F12 88.6(7) . . ? F10 P2 F12 176.0(8) . . ? F7 P2 F12 84.7(6) . . ? F11 P2 F12 86.7(4) . . ? F9 P2 F12 93.2(5) . . ? N2 C1 N1 104.1(5) . . ? N2 C1 Ag1 134.4(4) . . ? N1 C1 Ag1 121.2(4) . . ? C3 C2 N2 107.8(5) . . ? C3 C2 H2 126.1 . . ? N2 C2 H2 126.1 . . ? C2 C3 N1 106.6(6) . . ? C2 C3 H3 126.7 . . ? N1 C3 H3 126.7 . . ? N3 C4 N4 128.4(6) . . ? N3 C4 N1 116.6(6) . . ? N4 C4 N1 115.0(5) . . ? N4 C5 C6 122.3(7) . . ? N4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C7 C6 C5 117.6(7) . . ? C7 C6 H6 121.2 . . ? C5 C6 H6 121.2 . . ? N3 C7 C6 122.0(7) . . ? N3 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? N2 C8 C9 112.4(5) . . ? N2 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N2 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N5 C9 C10 120.8(6) . . ? N5 C9 C8 117.9(5) . . ? C10 C9 C8 121.3(6) . . ? C11 C10 C9 120.2(6) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 119.1(6) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 118.6(7) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 N5 123.5(6) . . ? C12 C13 H13 118.3 . . ? N5 C13 H13 118.3 . . ? N7 C14 N6 104.8(5) . . ? N7 C14 Ag2 133.2(5) . . ? N6 C14 Ag2 122.0(4) . . ? C16 C15 N7 107.6(6) . . ? C16 C15 H15 126.2 . . ? N7 C15 H15 126.2 . . ? C15 C16 N6 106.1(6) . . ? C15 C16 H16 126.9 . . ? N6 C16 H16 126.9 . . ? N9 C17 N8 127.8(7) . . ? N9 C17 N6 115.6(6) . . ? N8 C17 N6 116.7(6) . . ? C19 C18 N9 124.2(9) . . ? C19 C18 H18 117.9 . . ? N9 C18 H18 117.9 . . ? C18 C19 C20 116.4(9) . . ? C18 C19 H19 121.8 . . ? C20 C19 H19 121.8 . . ? N8 C20 C19 121.6(9) . . ? N8 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? N7 C21 C22 113.5(6) . . ? N7 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? N7 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? N10 C22 C23 120.9(6) . . ? N10 C22 C21 117.9(5) . . ? C23 C22 C21 121.2(6) . . ? C22 C23 C24 120.2(7) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.3(7) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 117.9(7) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? N10 C26 C25 122.6(7) . . ? N10 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? N11 C27 C28 179.2(14) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ag1 Ag2 C14 -128.2(3) . . . . ? N10 Ag1 Ag2 C14 56.1(2) . . . . ? C1 Ag1 Ag2 N5 50.2(2) . . . . ? N10 Ag1 Ag2 N5 -125.4(2) . . . . ? C14 Ag2 N5 C9 124(6) . . . . ? Ag1 Ag2 N5 C9 -12.7(5) . . . . ? C14 Ag2 N5 C13 -48(6) . . . . ? Ag1 Ag2 N5 C13 175.4(4) . . . . ? C1 Ag1 N10 C26 45(3) . . . . ? Ag2 Ag1 N10 C26 166.5(5) . . . . ? C1 Ag1 N10 C22 -129(2) . . . . ? Ag2 Ag1 N10 C22 -7.6(5) . . . . ? C2 N2 C1 N1 0.1(6) . . . . ? C8 N2 C1 N1 -178.0(5) . . . . ? C2 N2 C1 Ag1 174.6(5) . . . . ? C8 N2 C1 Ag1 -3.5(8) . . . . ? C3 N1 C1 N2 0.1(6) . . . . ? C4 N1 C1 N2 178.1(5) . . . . ? C3 N1 C1 Ag1 -175.3(4) . . . . ? C4 N1 C1 Ag1 2.7(7) . . . . ? N10 Ag1 C1 N2 62(3) . . . . ? Ag2 Ag1 C1 N2 -61.4(5) . . . . ? N10 Ag1 C1 N1 -124(2) . . . . ? Ag2 Ag1 C1 N1 112.4(4) . . . . ? C1 N2 C2 C3 -0.2(7) . . . . ? C8 N2 C2 C3 177.9(6) . . . . ? N2 C2 C3 N1 0.2(7) . . . . ? C1 N1 C3 C2 -0.2(7) . . . . ? C4 N1 C3 C2 -178.2(6) . . . . ? C7 N3 C4 N4 -3.1(10) . . . . ? C7 N3 C4 N1 179.9(6) . . . . ? C5 N4 C4 N3 1.6(10) . . . . ? C5 N4 C4 N1 178.7(6) . . . . ? C1 N1 C4 N3 0.8(8) . . . . ? C3 N1 C4 N3 178.6(6) . . . . ? C1 N1 C4 N4 -176.6(5) . . . . ? C3 N1 C4 N4 1.2(9) . . . . ? C4 N4 C5 C6 0.8(11) . . . . ? N4 C5 C6 C7 -1.4(13) . . . . ? C4 N3 C7 C6 2.3(11) . . . . ? C5 C6 C7 N3 -0.3(13) . . . . ? C1 N2 C8 C9 118.0(6) . . . . ? C2 N2 C8 C9 -59.8(7) . . . . ? C13 N5 C9 C10 -0.3(9) . . . . ? Ag2 N5 C9 C10 -172.2(5) . . . . ? C13 N5 C9 C8 -179.1(6) . . . . ? Ag2 N5 C9 C8 9.0(8) . . . . ? N2 C8 C9 N5 -70.0(7) . . . . ? N2 C8 C9 C10 111.2(7) . . . . ? N5 C9 C10 C11 0.7(11) . . . . ? C8 C9 C10 C11 179.5(7) . . . . ? C9 C10 C11 C12 -1.0(12) . . . . ? C10 C11 C12 C13 0.8(12) . . . . ? C11 C12 C13 N5 -0.4(12) . . . . ? C9 N5 C13 C12 0.1(10) . . . . ? Ag2 N5 C13 C12 172.5(6) . . . . ? C15 N7 C14 N6 -1.3(6) . . . . ? C21 N7 C14 N6 -173.7(5) . . . . ? C15 N7 C14 Ag2 175.1(5) . . . . ? C21 N7 C14 Ag2 2.7(9) . . . . ? C16 N6 C14 N7 1.6(6) . . . . ? C17 N6 C14 N7 177.2(5) . . . . ? C16 N6 C14 Ag2 -175.3(4) . . . . ? C17 N6 C14 Ag2 0.3(8) . . . . ? N5 Ag2 C14 N7 149(6) . . . . ? Ag1 Ag2 C14 N7 -73.3(5) . . . . ? N5 Ag2 C14 N6 -35(6) . . . . ? Ag1 Ag2 C14 N6 102.6(5) . . . . ? C14 N7 C15 C16 0.5(7) . . . . ? C21 N7 C15 C16 172.8(6) . . . . ? N7 C15 C16 N6 0.5(7) . . . . ? C14 N6 C16 C15 -1.4(7) . . . . ? C17 N6 C16 C15 -177.0(6) . . . . ? C18 N9 C17 N8 -1.0(12) . . . . ? C18 N9 C17 N6 178.1(8) . . . . ? C20 N8 C17 N9 1.1(11) . . . . ? C20 N8 C17 N6 -178.0(6) . . . . ? C14 N6 C17 N9 -178.3(6) . . . . ? C16 N6 C17 N9 -3.3(9) . . . . ? C14 N6 C17 N8 1.0(9) . . . . ? C16 N6 C17 N8 176.0(6) . . . . ? C17 N9 C18 C19 -0.3(16) . . . . ? N9 C18 C19 C20 1.2(17) . . . . ? C17 N8 C20 C19 0.0(12) . . . . ? C18 C19 C20 N8 -1.1(15) . . . . ? C14 N7 C21 C22 112.6(7) . . . . ? C15 N7 C21 C22 -58.7(8) . . . . ? C26 N10 C22 C23 -1.2(10) . . . . ? Ag1 N10 C22 C23 172.7(5) . . . . ? C26 N10 C22 C21 179.1(6) . . . . ? Ag1 N10 C22 C21 -7.0(8) . . . . ? N7 C21 C22 N10 -52.0(8) . . . . ? N7 C21 C22 C23 128.3(7) . . . . ? N10 C22 C23 C24 -0.4(12) . . . . ? C21 C22 C23 C24 179.3(8) . . . . ? C22 C23 C24 C25 1.5(14) . . . . ? C23 C24 C25 C26 -1.1(14) . . . . ? C22 N10 C26 C25 1.6(11) . . . . ? Ag1 N10 C26 C25 -172.9(7) . . . . ? C24 C25 C26 N10 -0.4(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.691 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.091 #===END data_071115b _database_code_depnum_ccdc_archive 'CCDC 675963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H31 F12 N9 P2 Pd' _chemical_formula_weight 841.94 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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 9.4669(10) _cell_length_b 24.487(2) _cell_length_c 14.7736(16) _cell_angle_alpha 90.00 _cell_angle_beta 101.008(2) _cell_angle_gamma 90.00 _cell_volume 3361.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7855 _exptl_absorpt_correction_T_max 0.9158 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 16800 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5928 _reflns_number_gt 4257 _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^)+(0.0760P)^2^+9.6850P] 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 5928 _refine_ls_number_parameters 436 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1787 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.34278(6) 0.18194(2) 0.78748(3) 0.0482(2) Uani 1 1 d . . . N1 N 0.2804(6) 0.1408(2) 0.8961(3) 0.0469(12) Uani 1 1 d . . . N2 N 0.4991(6) 0.1016(2) 0.8987(4) 0.0553(14) Uani 1 1 d . . . N3 N 0.6393(7) 0.1216(2) 0.8061(4) 0.0625(16) Uani 1 1 d . . . N4 N 0.2144(7) 0.1327(3) 0.6242(4) 0.0687(17) Uani 1 1 d . . . N5 N 0.2540(9) 0.1478(3) 0.4722(4) 0.082(2) Uani 1 1 d . . . N6 N 0.3573(6) 0.2037(3) 0.5918(4) 0.0584(15) Uani 1 1 d . . . N7 N 0.4849(7) 0.2622(3) 0.6777(4) 0.0643(16) Uani 1 1 d . . . N8 N 0.1745(7) 0.2361(2) 0.7704(4) 0.0573(15) Uani 1 1 d . . . N9 N 0.3631(8) 0.0704(2) 1.0043(4) 0.0676(17) Uani 1 1 d . . . C1 C 0.5129(7) 0.1338(3) 0.8242(5) 0.0515(16) Uani 1 1 d . . . C2 C 0.7085(9) 0.0823(3) 0.8675(6) 0.078(2) Uani 1 1 d . . . H7 H 0.7993 0.0675 0.8683 0.094 Uiso 1 1 calc R . . C3 C 0.6206(9) 0.0699(3) 0.9244(6) 0.072(2) Uani 1 1 d . . . H8 H 0.6375 0.0448 0.9724 0.086 Uiso 1 1 calc R . . C4 C 0.3758(8) 0.1034(3) 0.9361(4) 0.0510(16) Uani 1 1 d . . . C5 C 0.2396(11) 0.0751(3) 1.0339(5) 0.074(2) Uani 1 1 d . . . H3 H 0.2241 0.0522 1.0813 0.089 Uiso 1 1 calc R . . C6 C 0.1345(10) 0.1114(3) 0.9992(5) 0.069(2) Uani 1 1 d . . . H4 H 0.0499 0.1137 1.0222 0.083 Uiso 1 1 calc R . . C7 C 0.1586(9) 0.1445(3) 0.9285(5) 0.0606(18) Uani 1 1 d . . . H5 H 0.0891 0.1699 0.9030 0.073 Uiso 1 1 calc R . . C8 C 0.7039(10) 0.1438(4) 0.7324(7) 0.090(3) Uani 1 1 d D . . H8A H 0.6369 0.1703 0.6993 0.108 Uiso 1 1 calc R . . H8B H 0.7893 0.1639 0.7609 0.108 Uiso 1 1 calc R . . C12 C 0.4038(7) 0.2183(3) 0.6810(4) 0.0489(15) Uani 1 1 d . . . C13 C 0.4910(10) 0.2748(4) 0.5867(6) 0.077(2) Uani 1 1 d . . . H19 H 0.5424 0.3034 0.5669 0.092 Uiso 1 1 calc R . . C14 C 0.4117(10) 0.2394(4) 0.5344(6) 0.077(2) Uani 1 1 d . . . H20 H 0.3947 0.2382 0.4703 0.092 Uiso 1 1 calc R . . C15 C 0.2675(8) 0.1577(3) 0.5608(5) 0.0585(18) Uani 1 1 d . . . C16 C 0.1302(11) 0.0899(4) 0.5936(7) 0.093(3) Uani 1 1 d . . . H17 H 0.0897 0.0696 0.6354 0.112 Uiso 1 1 calc R . . C17 C 0.1024(13) 0.0752(4) 0.5024(8) 0.106(3) Uani 1 1 d . . . H16 H 0.0410 0.0464 0.4810 0.127 Uiso 1 1 calc R . . C18 C 0.1676(13) 0.1043(5) 0.4457(7) 0.103(3) Uani 1 1 d . . . H15 H 0.1528 0.0940 0.3841 0.123 Uiso 1 1 calc R . . C23 C 0.0905(8) 0.2690(3) 0.7620(5) 0.0585(18) Uani 1 1 d . . . C24 C -0.0116(11) 0.3137(4) 0.7503(6) 0.086(3) Uani 1 1 d . . . H26A H -0.0066 0.3323 0.8080 0.130 Uiso 1 1 calc R . . H26B H -0.1070 0.2996 0.7298 0.130 Uiso 1 1 calc R . . H26C H 0.0111 0.3387 0.7052 0.130 Uiso 1 1 calc R . . C25 C 0.744(2) 0.1081(7) 0.6657(11) 0.226(12) Uani 1 1 d D . . H25A H 0.7996 0.0780 0.6974 0.271 Uiso 1 1 calc R . . H25B H 0.8065 0.1278 0.6317 0.271 Uiso 1 1 calc R . . C26 C 0.620(3) 0.0857(10) 0.5993(18) 0.275(15) Uani 1 1 d D . . H26D H 0.5615 0.1155 0.5699 0.329 Uiso 1 1 calc R . . H26E H 0.5615 0.0637 0.6324 0.329 Uiso 1 1 calc R . . C27 C 0.671(2) 0.0503(9) 0.5249(13) 0.243(11) Uani 1 1 d D . . H27A H 0.7488 0.0682 0.5041 0.364 Uiso 1 1 calc R . . H27B H 0.5922 0.0454 0.4738 0.364 Uiso 1 1 calc R . . H27C H 0.7020 0.0153 0.5505 0.364 Uiso 1 1 calc R . . C28 C 0.5642(12) 0.2912(4) 0.7585(7) 0.099(3) Uani 1 1 d D . . H28A H 0.5188 0.2830 0.8104 0.119 Uiso 1 1 calc R . . H28B H 0.6609 0.2764 0.7725 0.119 Uiso 1 1 calc R . . C29 C 0.576(3) 0.3506(6) 0.7518(15) 0.272(15) Uani 1 1 d D . . H29A H 0.5949 0.3602 0.6916 0.327 Uiso 1 1 calc R . . H29B H 0.6556 0.3634 0.7980 0.327 Uiso 1 1 calc R . . C31 C 0.442(3) 0.3782(8) 0.7653(16) 0.244(12) Uani 1 1 d D . . H31A H 0.4173 0.3663 0.8231 0.292 Uiso 1 1 calc R . . H31B H 0.3631 0.3683 0.7157 0.292 Uiso 1 1 calc R . . C32 C 0.463(2) 0.4418(6) 0.7668(12) 0.197(8) Uani 1 1 d D . . H32A H 0.5216 0.4525 0.8246 0.295 Uiso 1 1 calc R . . H32B H 0.3715 0.4596 0.7592 0.295 Uiso 1 1 calc R . . H32C H 0.5105 0.4523 0.7173 0.295 Uiso 1 1 calc R . . P1 P 0.8622(3) 0.24910(11) 0.99407(17) 0.0800(7) Uani 1 1 d . . . F1 F 0.8322(8) 0.2674(3) 1.0904(4) 0.129(2) Uani 1 1 d . . . F2 F 0.8859(7) 0.2289(3) 0.8959(4) 0.115(2) Uani 1 1 d . . . F3 F 0.8444(11) 0.1893(3) 1.0219(5) 0.156(3) Uani 1 1 d . . . F4 F 1.0238(7) 0.2424(4) 1.0325(6) 0.179(4) Uani 1 1 d . . . F5 F 0.8753(15) 0.3079(3) 0.9618(8) 0.220(6) Uani 1 1 d . . . F6 F 0.6994(8) 0.2530(5) 0.9550(5) 0.207(5) Uani 1 1 d . . . P2 P 0.9212(3) 0.02149(10) 0.19449(16) 0.0765(6) Uani 1 1 d . . . F7 F 0.9914(13) -0.0333(4) 0.2014(9) 0.229(5) Uani 1 1 d . . . F8 F 0.8429(11) 0.0753(3) 0.1764(10) 0.229(5) Uani 1 1 d . . . F9 F 0.7824(10) -0.0117(4) 0.1831(7) 0.190(4) Uani 1 1 d . . . F10 F 0.9222(12) 0.0286(5) 0.2951(5) 0.218(5) Uani 1 1 d . . . F11 F 1.0613(8) 0.0564(4) 0.2051(5) 0.162(3) Uani 1 1 d . . . F12 F 0.9241(13) 0.0157(4) 0.0905(5) 0.213(5) 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 Pd1 0.0547(3) 0.0504(3) 0.0393(3) 0.0066(2) 0.0085(2) 0.0076(2) N1 0.058(3) 0.046(3) 0.037(3) 0.001(2) 0.010(2) 0.003(3) N2 0.060(4) 0.051(3) 0.053(3) 0.010(3) 0.005(3) 0.010(3) N3 0.057(4) 0.057(4) 0.076(4) 0.003(3) 0.020(3) 0.012(3) N4 0.072(4) 0.079(4) 0.054(4) 0.004(3) 0.010(3) -0.015(4) N5 0.112(6) 0.084(5) 0.049(4) -0.002(3) 0.012(4) 0.009(5) N6 0.060(4) 0.070(4) 0.049(3) 0.012(3) 0.018(3) 0.009(3) N7 0.056(4) 0.066(4) 0.070(4) 0.015(3) 0.011(3) 0.002(3) N8 0.067(4) 0.056(4) 0.053(3) 0.013(3) 0.020(3) 0.010(3) N9 0.087(5) 0.059(4) 0.057(4) 0.020(3) 0.015(3) 0.005(3) C1 0.053(4) 0.047(4) 0.053(4) 0.002(3) 0.006(3) 0.004(3) C2 0.060(5) 0.071(5) 0.100(7) 0.018(5) 0.008(5) 0.021(4) C3 0.072(5) 0.070(5) 0.069(5) 0.019(4) 0.001(4) 0.016(4) C4 0.062(4) 0.042(3) 0.045(4) 0.001(3) 0.001(3) 0.000(3) C5 0.110(7) 0.061(5) 0.054(5) 0.010(4) 0.020(5) -0.009(5) C6 0.092(6) 0.067(5) 0.053(4) 0.005(4) 0.028(4) 0.000(4) C7 0.073(5) 0.057(4) 0.054(4) 0.002(3) 0.017(4) 0.012(4) C8 0.067(5) 0.106(7) 0.103(7) 0.012(6) 0.036(5) 0.021(5) C12 0.043(4) 0.057(4) 0.047(4) 0.008(3) 0.010(3) 0.011(3) C13 0.081(6) 0.077(6) 0.079(6) 0.025(5) 0.033(5) -0.002(5) C14 0.097(6) 0.082(6) 0.059(5) 0.022(4) 0.036(5) 0.004(5) C15 0.063(5) 0.069(5) 0.043(4) 0.001(3) 0.007(3) 0.005(4) C16 0.101(7) 0.093(7) 0.084(7) 0.006(5) 0.013(5) -0.026(6) C17 0.135(10) 0.092(7) 0.083(7) -0.021(6) 0.002(7) -0.027(7) C18 0.126(9) 0.110(8) 0.065(6) -0.016(6) -0.001(6) 0.014(7) C23 0.067(5) 0.056(4) 0.052(4) 0.011(3) 0.013(3) 0.008(4) C24 0.100(7) 0.090(6) 0.070(5) 0.012(5) 0.018(5) 0.040(5) C25 0.39(3) 0.172(17) 0.152(15) 0.072(13) 0.131(19) 0.16(2) C26 0.29(3) 0.22(2) 0.28(3) -0.11(2) -0.03(2) 0.07(2) C27 0.32(3) 0.24(2) 0.161(17) -0.065(16) 0.045(18) 0.06(2) C28 0.100(7) 0.087(7) 0.103(8) 0.004(6) 0.002(6) -0.023(6) C29 0.48(5) 0.098(12) 0.21(2) -0.034(13) 0.00(3) 0.00(2) C31 0.33(3) 0.20(2) 0.25(2) 0.093(18) 0.15(2) 0.11(2) C32 0.28(2) 0.103(11) 0.200(17) 0.026(11) 0.023(15) 0.059(13) P1 0.0825(16) 0.0847(16) 0.0751(15) 0.0081(12) 0.0212(12) 0.0202(13) F1 0.186(7) 0.127(5) 0.080(4) -0.005(3) 0.037(4) 0.050(5) F2 0.115(5) 0.152(6) 0.086(4) 0.001(4) 0.035(3) 0.028(4) F3 0.261(10) 0.096(5) 0.111(5) -0.003(4) 0.036(6) -0.022(5) F4 0.093(5) 0.258(10) 0.173(7) -0.086(7) -0.009(5) 0.026(6) F5 0.389(17) 0.107(6) 0.216(10) 0.037(6) 0.188(11) 0.043(8) F6 0.102(5) 0.431(16) 0.091(5) 0.051(7) 0.030(4) 0.090(8) P2 0.0924(17) 0.0684(14) 0.0703(14) -0.0073(11) 0.0197(12) -0.0069(12) F7 0.237(11) 0.169(9) 0.287(14) 0.013(8) 0.065(10) 0.108(8) F8 0.194(10) 0.103(6) 0.381(17) 0.017(8) 0.034(10) 0.015(6) F9 0.177(8) 0.188(8) 0.223(9) -0.099(7) 0.082(7) -0.115(7) F10 0.305(12) 0.280(12) 0.082(5) -0.067(6) 0.074(6) -0.175(10) F11 0.130(6) 0.228(9) 0.142(6) -0.055(6) 0.057(5) -0.078(6) F12 0.336(13) 0.212(9) 0.102(5) -0.035(6) 0.069(7) -0.143(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.987(7) . ? Pd1 C12 1.987(7) . ? Pd1 N8 2.051(6) . ? Pd1 N1 2.074(5) . ? Pd1 N4 2.762(6) . ? N1 C7 1.333(9) . ? N1 C4 1.343(8) . ? N2 C1 1.379(8) . ? N2 C3 1.379(9) . ? N2 C4 1.384(9) . ? N3 C1 1.309(9) . ? N3 C2 1.398(9) . ? N3 C8 1.453(10) . ? N4 C15 1.299(9) . ? N4 C16 1.343(11) . ? N5 C15 1.313(9) . ? N5 C18 1.354(13) . ? N6 C12 1.356(8) . ? N6 C14 1.382(9) . ? N6 C15 1.432(10) . ? N7 C12 1.328(9) . ? N7 C13 1.391(10) . ? N7 C28 1.466(11) . ? N8 C23 1.122(8) . ? N9 C4 1.314(8) . ? N9 C5 1.330(11) . ? C2 C3 1.326(11) . ? C2 H7 0.9300 . ? C3 H8 0.9300 . ? C5 C6 1.359(11) . ? C5 H3 0.9300 . ? C6 C7 1.375(10) . ? C6 H4 0.9300 . ? C7 H5 0.9300 . ? C8 C25 1.424(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C13 C14 1.302(12) . ? C13 H19 0.9300 . ? C14 H20 0.9300 . ? C16 C17 1.370(13) . ? C16 H17 0.9300 . ? C17 C18 1.338(15) . ? C17 H16 0.9300 . ? C18 H15 0.9300 . ? C23 C24 1.447(11) . ? C24 H26A 0.9600 . ? C24 H26B 0.9600 . ? C24 H26C 0.9600 . ? C25 C26 1.485(17) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.545(16) . ? C26 H26D 0.9700 . ? C26 H26E 0.9700 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.464(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C31 1.482(17) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C31 C32 1.572(16) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? P1 F5 1.530(8) . ? P1 F4 1.536(7) . ? P1 F3 1.539(7) . ? P1 F6 1.542(7) . ? P1 F1 1.568(6) . ? P1 F2 1.588(6) . ? P2 F7 1.492(9) . ? P2 F10 1.495(7) . ? P2 F8 1.512(9) . ? P2 F9 1.527(7) . ? P2 F12 1.548(8) . ? P2 F11 1.560(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C12 98.0(3) . . ? C1 Pd1 N8 171.0(3) . . ? C12 Pd1 N8 87.1(2) . . ? C1 Pd1 N1 80.6(3) . . ? C12 Pd1 N1 177.6(2) . . ? N8 Pd1 N1 94.6(2) . . ? C1 Pd1 N4 100.3(2) . . ? C12 Pd1 N4 69.5(2) . . ? N8 Pd1 N4 88.5(2) . . ? N1 Pd1 N4 108.7(2) . . ? C7 N1 C4 116.3(6) . . ? C7 N1 Pd1 129.7(5) . . ? C4 N1 Pd1 113.9(5) . . ? C1 N2 C3 109.9(6) . . ? C1 N2 C4 121.1(6) . . ? C3 N2 C4 129.0(6) . . ? C1 N3 C2 110.9(7) . . ? C1 N3 C8 126.9(6) . . ? C2 N3 C8 122.2(7) . . ? C15 N4 C16 114.4(7) . . ? C15 N4 Pd1 104.9(5) . . ? C16 N4 Pd1 140.3(6) . . ? C15 N5 C18 111.9(8) . . ? C12 N6 C14 109.9(7) . . ? C12 N6 C15 125.5(6) . . ? C14 N6 C15 124.6(7) . . ? C12 N7 C13 110.3(7) . . ? C12 N7 C28 124.9(7) . . ? C13 N7 C28 124.7(7) . . ? C23 N8 Pd1 174.4(6) . . ? C4 N9 C5 114.5(7) . . ? N3 C1 N2 105.3(6) . . ? N3 C1 Pd1 143.5(5) . . ? N2 C1 Pd1 111.2(5) . . ? C3 C2 N3 107.2(7) . . ? C3 C2 H7 126.4 . . ? N3 C2 H7 126.4 . . ? C2 C3 N2 106.8(7) . . ? C2 C3 H8 126.6 . . ? N2 C3 H8 126.6 . . ? N9 C4 N1 127.2(7) . . ? N9 C4 N2 119.6(6) . . ? N1 C4 N2 113.2(6) . . ? N9 C5 C6 123.9(7) . . ? N9 C5 H3 118.0 . . ? C6 C5 H3 118.0 . . ? C5 C6 C7 117.2(8) . . ? C5 C6 H4 121.4 . . ? C7 C6 H4 121.4 . . ? N1 C7 C6 120.8(7) . . ? N1 C7 H5 119.6 . . ? C6 C7 H5 119.6 . . ? C25 C8 N3 119.7(11) . . ? C25 C8 H8A 107.4 . . ? N3 C8 H8A 107.4 . . ? C25 C8 H8B 107.4 . . ? N3 C8 H8B 107.4 . . ? H8A C8 H8B 106.9 . . ? N7 C12 N6 105.1(6) . . ? N7 C12 Pd1 130.5(5) . . ? N6 C12 Pd1 124.2(5) . . ? C14 C13 N7 107.4(7) . . ? C14 C13 H19 126.3 . . ? N7 C13 H19 126.3 . . ? C13 C14 N6 107.3(7) . . ? C13 C14 H20 126.3 . . ? N6 C14 H20 126.3 . . ? N4 C15 N5 130.9(8) . . ? N4 C15 N6 115.4(6) . . ? N5 C15 N6 113.7(7) . . ? N4 C16 C17 121.7(9) . . ? N4 C16 H17 119.1 . . ? C17 C16 H17 119.1 . . ? C18 C17 C16 116.8(10) . . ? C18 C17 H16 121.6 . . ? C16 C17 H16 121.6 . . ? C17 C18 N5 124.3(9) . . ? C17 C18 H15 117.8 . . ? N5 C18 H15 117.8 . . ? N8 C23 C24 176.8(9) . . ? C23 C24 H26A 109.5 . . ? C23 C24 H26B 109.5 . . ? H26A C24 H26B 109.5 . . ? C23 C24 H26C 109.5 . . ? H26A C24 H26C 109.5 . . ? H26B C24 H26C 109.5 . . ? C8 C25 C26 113.6(16) . . ? C8 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? C8 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C25 C26 C27 111.4(18) . . ? C25 C26 H26D 109.4 . . ? C27 C26 H26D 109.4 . . ? C25 C26 H26E 109.4 . . ? C27 C26 H26E 109.4 . . ? H26D C26 H26E 108.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 N7 117.3(11) . . ? C29 C28 H28A 108.0 . . ? N7 C28 H28A 108.0 . . ? C29 C28 H28B 108.0 . . ? N7 C28 H28B 108.0 . . ? H28A C28 H28B 107.2 . . ? C28 C29 C31 111.6(18) . . ? C28 C29 H29A 109.3 . . ? C31 C29 H29A 109.3 . . ? C28 C29 H29B 109.3 . . ? C31 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C29 C31 C32 109.9(16) . . ? C29 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? C29 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? F5 P1 F4 94.7(7) . . ? F5 P1 F3 177.2(6) . . ? F4 P1 F3 87.3(6) . . ? F5 P1 F6 87.7(7) . . ? F4 P1 F6 177.4(6) . . ? F3 P1 F6 90.4(6) . . ? F5 P1 F1 93.1(5) . . ? F4 P1 F1 92.0(4) . . ? F3 P1 F1 88.9(4) . . ? F6 P1 F1 88.9(4) . . ? F5 P1 F2 88.5(5) . . ? F4 P1 F2 90.0(4) . . ? F3 P1 F2 89.4(4) . . ? F6 P1 F2 89.0(4) . . ? F1 P1 F2 177.3(4) . . ? F7 P2 F10 96.8(7) . . ? F7 P2 F8 173.6(7) . . ? F10 P2 F8 89.0(7) . . ? F7 P2 F9 83.8(6) . . ? F10 P2 F9 90.8(5) . . ? F8 P2 F9 93.5(6) . . ? F7 P2 F12 83.9(7) . . ? F10 P2 F12 178.0(5) . . ? F8 P2 F12 90.3(7) . . ? F9 P2 F12 91.1(5) . . ? F7 P2 F11 97.3(6) . . ? F10 P2 F11 89.6(4) . . ? F8 P2 F11 85.4(5) . . ? F9 P2 F11 178.8(6) . . ? F12 P2 F11 88.5(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.989 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.097 #===END data_071211d _database_code_depnum_ccdc_archive 'CCDC 675964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 F12 N12 P2 Pd' _chemical_formula_weight 952.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _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 20.944(2) _cell_length_b 12.8532(13) _cell_length_c 14.2227(18) _cell_angle_alpha 90.00 _cell_angle_beta 96.152(2) _cell_angle_gamma 90.00 _cell_volume 3806.7(7) _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 Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8829 _exptl_absorpt_correction_T_max 0.9237 _exptl_absorpt_process_details Sadabs _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 9235 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3352 _reflns_number_gt 2488 _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^)+(0.1178P)^2^+15.6783P] 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 3352 _refine_ls_number_parameters 258 _refine_ls_number_restraints 158 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.2169 _refine_ls_wR_factor_gt 0.1809 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.174 _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 Pd1 Pd 0.5000 0.36910(6) 0.7500 0.0391(3) Uani 1 2 d S . . P1 P 0.69020(12) 0.6448(2) 0.85214(19) 0.0728(8) Uani 1 1 d U . . F1 F 0.6578(3) 0.5343(5) 0.8456(6) 0.112(2) Uani 1 1 d U . . F2 F 0.7214(4) 0.7549(7) 0.8598(7) 0.153(3) Uani 1 1 d U . . F3 F 0.6453(5) 0.6737(7) 0.9283(7) 0.150(3) Uani 1 1 d U . . F4 F 0.7391(5) 0.6068(7) 0.9323(8) 0.156(3) Uani 1 1 d U . . F5 F 0.7324(6) 0.6134(9) 0.7783(9) 0.190(4) Uani 1 1 d U . . F6 F 0.6377(4) 0.6836(8) 0.7756(7) 0.148(3) Uani 1 1 d U . . N1 N 0.4086(3) 0.2754(4) 0.8620(4) 0.0374(12) Uani 1 1 d . . . N2 N 0.4887(3) 0.1710(4) 0.8680(4) 0.0426(14) Uani 1 1 d . . . N3 N 0.4640(2) 0.4796(4) 0.8382(4) 0.0344(12) Uani 1 1 d . . . N4 N 0.5966(3) 0.1846(6) 0.8470(5) 0.0634(19) Uani 1 1 d . . . N5 N 0.5474(5) 0.0189(7) 0.8666(6) 0.086(3) Uani 1 1 d . . . N6 N 0.5940(14) 0.8764(16) 0.583(2) 0.224(9) Uani 1 1 d DU . . C1 C 0.4671(3) 0.2637(5) 0.8323(4) 0.0355(14) Uani 1 1 d . . . C2 C 0.4412(4) 0.1250(6) 0.9178(6) 0.056(2) Uani 1 1 d . . . H2 H 0.4438 0.0607 0.9480 0.068 Uiso 1 1 calc R . . C3 C 0.3923(4) 0.1908(6) 0.9134(6) 0.0526(19) Uani 1 1 d . . . H3 H 0.3541 0.1814 0.9402 0.063 Uiso 1 1 calc R . . C4 C 0.3695(3) 0.3689(5) 0.8390(5) 0.0412(15) Uani 1 1 d . . . H4A H 0.3304 0.3652 0.8698 0.049 Uiso 1 1 calc R . . H4B H 0.3576 0.3723 0.7713 0.049 Uiso 1 1 calc R . . C5 C 0.4066(3) 0.4645(5) 0.8712(4) 0.0360(14) Uani 1 1 d . . . C6 C 0.3837(4) 0.5342(6) 0.9331(5) 0.0513(19) Uani 1 1 d . . . H6 H 0.3435 0.5240 0.9537 0.062 Uiso 1 1 calc R . . C7 C 0.4201(5) 0.6190(6) 0.9647(6) 0.060(2) Uani 1 1 d . . . H7 H 0.4057 0.6653 1.0081 0.072 Uiso 1 1 calc R . . C8 C 0.4779(5) 0.6333(7) 0.9308(6) 0.060(2) Uani 1 1 d . . . H8 H 0.5032 0.6905 0.9501 0.072 Uiso 1 1 calc R . . C9 C 0.4985(3) 0.5634(6) 0.8685(5) 0.0457(17) Uani 1 1 d . . . H9 H 0.5381 0.5742 0.8461 0.055 Uiso 1 1 calc R . . C10 C 0.5490(4) 0.1229(6) 0.8603(5) 0.053(2) Uani 1 1 d . . . C11 C 0.6044(7) -0.0268(10) 0.8605(9) 0.111(5) Uani 1 1 d . . . H11 H 0.6075 -0.0987 0.8667 0.133 Uiso 1 1 calc R . . C12 C 0.6599(7) 0.0300(11) 0.8451(9) 0.106(5) Uani 1 1 d . . . H12 H 0.6992 -0.0018 0.8403 0.127 Uiso 1 1 calc R . . C13 C 0.6516(5) 0.1357(10) 0.8378(8) 0.088(4) Uani 1 1 d . . . H13 H 0.6868 0.1758 0.8256 0.106 Uiso 1 1 calc R . . C14 C 0.6504(13) 0.8709(19) 0.608(2) 0.214(10) Uani 1 1 d DU . . C15 C 0.7185(12) 0.8385(19) 0.593(2) 0.276(12) Uani 1 1 d DU . . H15A H 0.7171 0.7796 0.5516 0.413 Uiso 1 1 calc R . . H15B H 0.7413 0.8201 0.6532 0.413 Uiso 1 1 calc R . . H15C H 0.7400 0.8952 0.5662 0.413 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 Pd1 0.0353(4) 0.0496(5) 0.0339(4) 0.000 0.0102(3) 0.000 P1 0.0539(13) 0.101(2) 0.0654(15) -0.0129(13) 0.0152(11) -0.0185(13) F1 0.102(5) 0.098(5) 0.135(6) -0.038(4) 0.016(4) -0.015(4) F2 0.132(6) 0.140(7) 0.182(8) 0.011(6) -0.003(6) -0.071(5) F3 0.176(7) 0.142(6) 0.143(7) -0.059(6) 0.073(6) -0.022(6) F4 0.117(6) 0.158(7) 0.178(8) 0.035(6) -0.051(6) -0.028(5) F5 0.157(8) 0.236(10) 0.200(9) -0.019(7) 0.126(7) -0.009(7) F6 0.139(6) 0.150(7) 0.144(7) 0.030(6) -0.036(5) -0.011(6) N1 0.037(3) 0.039(3) 0.037(3) 0.001(2) 0.010(2) -0.003(2) N2 0.055(4) 0.041(3) 0.034(3) 0.002(2) 0.015(3) 0.007(3) N3 0.033(3) 0.041(3) 0.030(3) 0.002(2) 0.007(2) -0.002(2) N4 0.044(4) 0.083(5) 0.065(5) 0.010(4) 0.013(3) 0.015(4) N5 0.106(7) 0.076(6) 0.084(6) 0.021(4) 0.046(5) 0.035(5) N6 0.28(2) 0.155(14) 0.225(17) 0.013(11) -0.014(18) 0.034(15) C1 0.040(4) 0.044(4) 0.023(3) -0.003(3) 0.008(3) 0.004(3) C2 0.068(5) 0.049(4) 0.055(5) 0.010(4) 0.025(4) -0.003(4) C3 0.057(5) 0.048(4) 0.056(5) 0.008(4) 0.021(4) -0.008(4) C4 0.028(3) 0.049(4) 0.049(4) 0.000(3) 0.013(3) 0.000(3) C5 0.031(3) 0.042(4) 0.035(3) 0.006(3) 0.007(3) 0.007(3) C6 0.052(4) 0.057(5) 0.046(4) 0.004(4) 0.015(3) 0.016(4) C7 0.077(6) 0.060(5) 0.044(4) -0.007(4) 0.015(4) 0.016(4) C8 0.073(6) 0.058(5) 0.049(4) -0.012(4) 0.003(4) -0.007(4) C9 0.045(4) 0.057(4) 0.037(4) 0.001(3) 0.011(3) -0.006(3) C10 0.069(5) 0.056(5) 0.037(4) 0.013(3) 0.017(4) 0.024(4) C11 0.149(12) 0.087(8) 0.106(10) 0.034(7) 0.057(9) 0.061(8) C12 0.114(10) 0.123(11) 0.089(8) 0.031(7) 0.043(7) 0.071(9) C13 0.061(6) 0.132(11) 0.076(7) 0.022(6) 0.028(5) 0.036(6) C14 0.26(2) 0.145(15) 0.24(2) 0.019(14) 0.03(2) 0.067(18) C15 0.26(2) 0.193(18) 0.35(2) 0.144(17) -0.11(2) -0.030(18) _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 Pd1 C1 1.963(6) 2_656 ? Pd1 C1 1.963(6) . ? Pd1 N3 2.088(5) 2_656 ? Pd1 N3 2.088(5) . ? P1 F5 1.498(9) . ? P1 F4 1.529(9) . ? P1 F6 1.544(8) . ? P1 F3 1.552(8) . ? P1 F2 1.558(8) . ? P1 F1 1.573(7) . ? N1 C1 1.347(8) . ? N1 C3 1.373(9) . ? N1 C4 1.471(8) . ? N2 C1 1.355(8) . ? N2 C2 1.410(9) . ? N2 C10 1.422(10) . ? N3 C9 1.342(9) . ? N3 C5 1.351(8) . ? N4 C10 1.303(11) . ? N4 C13 1.332(11) . ? N5 C10 1.340(11) . ? N5 C11 1.342(14) . ? N6 C14 1.198(10) . ? C2 C3 1.325(12) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.499(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.378(10) . ? C6 C7 1.378(12) . ? C6 H6 0.9300 . ? C7 C8 1.362(13) . ? C7 H7 0.9300 . ? C8 C9 1.365(11) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C11 C12 1.408(19) . ? C11 H11 0.9300 . ? C12 C13 1.372(16) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.522(10) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 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 C1 Pd1 C1 92.7(4) 2_656 . ? C1 Pd1 N3 86.5(2) 2_656 2_656 ? C1 Pd1 N3 179.2(2) . 2_656 ? C1 Pd1 N3 179.2(2) 2_656 . ? C1 Pd1 N3 86.5(2) . . ? N3 Pd1 N3 94.3(3) 2_656 . ? F5 P1 F4 92.2(8) . . ? F5 P1 F6 91.2(7) . . ? F4 P1 F6 176.5(6) . . ? F5 P1 F3 178.1(6) . . ? F4 P1 F3 87.9(7) . . ? F6 P1 F3 88.6(6) . . ? F5 P1 F2 91.1(6) . . ? F4 P1 F2 89.7(5) . . ? F6 P1 F2 91.0(5) . . ? F3 P1 F2 90.8(5) . . ? F5 P1 F1 89.9(5) . . ? F4 P1 F1 90.4(5) . . ? F6 P1 F1 88.9(5) . . ? F3 P1 F1 88.2(4) . . ? F2 P1 F1 179.0(5) . . ? C1 N1 C3 111.4(6) . . ? C1 N1 C4 121.6(5) . . ? C3 N1 C4 127.0(6) . . ? C1 N2 C2 109.4(6) . . ? C1 N2 C10 128.1(6) . . ? C2 N2 C10 122.5(6) . . ? C9 N3 C5 118.2(6) . . ? C9 N3 Pd1 121.5(4) . . ? C5 N3 Pd1 120.2(4) . . ? C10 N4 C13 114.3(9) . . ? C10 N5 C11 113.8(10) . . ? N1 C1 N2 104.9(5) . . ? N1 C1 Pd1 120.0(5) . . ? N2 C1 Pd1 134.9(5) . . ? C3 C2 N2 107.0(7) . . ? C3 C2 H2 126.5 . . ? N2 C2 H2 126.5 . . ? C2 C3 N1 107.2(7) . . ? C2 C3 H3 126.4 . . ? N1 C3 H3 126.4 . . ? N1 C4 C5 110.1(5) . . ? N1 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? N1 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 120.8(6) . . ? N3 C5 C4 117.6(5) . . ? C6 C5 C4 121.6(6) . . ? C5 C6 C7 120.3(7) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C8 C7 C6 118.2(7) . . ? C8 C7 H7 120.9 . . ? C6 C7 H7 120.9 . . ? C7 C8 C9 119.7(8) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? N3 C9 C8 122.7(7) . . ? N3 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? N4 C10 N5 129.9(8) . . ? N4 C10 N2 116.5(7) . . ? N5 C10 N2 113.5(8) . . ? N5 C11 C12 122.5(11) . . ? N5 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 115.2(10) . . ? C13 C12 H12 122.4 . . ? C11 C12 H12 122.4 . . ? N4 C13 C12 124.2(11) . . ? N4 C13 H13 117.9 . . ? C12 C13 H13 117.9 . . ? N6 C14 C15 152(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.172 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.137 #===END