# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;A tiny tris(imidazolium) cage forms an N-heterocyclic carbene complex with silver(I) ; _publ_contact_author_name 'Jonathan Steed' _publ_contact_author_email JON.STEED@DURHAM.AC.UK loop_ _publ_author_name 'Jonathan Steed' 'Kirsty Anderson' 'L. Barbour' 'Peter C. Junk' 'Charlotte E. Willans' # Attachment '07srv070.CIF' data_c:\kirsty~1\crysta~1\charlo~1\07srv070\work\cewfe_m _database_code_depnum_ccdc_archive 'CCDC 650053' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H51 N6, 2(Cl4 Fe), Br' _chemical_formula_sum 'C39 H51 Br Cl8 Fe2 N6' _chemical_formula_weight 1079.07 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' N N 0.0061 0.0033 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P 21 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-y+1/2, -z, x+1/2' 'z+1/2, -x+1/2, -y' '-y, z+1/2, -x+1/2' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 16.6032(7) _cell_length_b 16.6032(7) _cell_length_c 16.6032(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4576.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'triangular plate' _exptl_crystal_colour orange _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 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 2.010 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; absorption correction increased R1 by ~ 1% ; _diffrn_ambient_temperature 120(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 'SMART 6k' _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 77681 _diffrn_reflns_av_R_equivalents 0.2321 _diffrn_reflns_av_sigmaI/netI 0.1230 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.15 _reflns_number_total 4143 _reflns_number_gt 2350 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-SEed _computing_publication_material X-seed _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^)+(0.0434P)^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 calc _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 0.048(15) _refine_ls_number_reflns 4143 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1027 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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 Br1 Br 0.78514(4) 0.78514(4) 0.78514(4) 0.0474(3) Uani 1 3 d S . . Fe1 Fe 0.25509(4) 0.25509(4) 0.25509(4) 0.0229(3) Uani 1 3 d S . . Fe2 Fe 0.05316(6) 0.44684(6) 0.55316(6) 0.0407(4) Uani 1 3 d S . . Cl1 Cl 0.22126(8) 0.31631(7) 0.14290(7) 0.0301(3) Uani 1 1 d . . . Cl2 Cl 0.33125(7) 0.33125(7) 0.33125(7) 0.0356(6) Uani 1 3 d S . . Cl3 Cl -0.02374(9) 0.52374(9) 0.47626(9) 0.0629(8) Uani 1 3 d S . . Cl4 Cl 0.13073(8) 0.52580(9) 0.62564(12) 0.0530(5) Uani 1 1 d . . . N5 N 0.4384(2) 0.5650(2) 0.7251(2) 0.0180(8) Uani 1 1 d . . . N9 N 0.3634(2) 0.4898(2) 0.6494(2) 0.0169(8) Uani 1 1 d . . . C1 C 0.4087(3) 0.2529(3) 0.5530(3) 0.0326(12) Uani 1 1 d . . . H1A H 0.3528 0.2674 0.5410 0.049 Uiso 1 1 calc R . . H1B H 0.4099 0.2152 0.5985 0.049 Uiso 1 1 calc R . . H1C H 0.4331 0.2274 0.5057 0.049 Uiso 1 1 calc R . . C2 C 0.4551(3) 0.3272(3) 0.5744(3) 0.0228(11) Uani 1 1 d . . . H2A H 0.4330 0.3501 0.6248 0.027 Uiso 1 1 calc R . . H2B H 0.5120 0.3124 0.5845 0.027 Uiso 1 1 calc R . . C3 C 0.4522(3) 0.3898(3) 0.5100(3) 0.0157(9) Uani 1 1 d . . . C4 C 0.3913(3) 0.4487(3) 0.5098(3) 0.0159(9) Uani 1 1 d . . . C5 C 0.3294(3) 0.4497(3) 0.5778(3) 0.0209(10) Uani 1 1 d . . . H5A H 0.2804 0.4786 0.5599 0.025 Uiso 1 1 calc R . . H5B H 0.3139 0.3938 0.5916 0.025 Uiso 1 1 calc R . . C6 C 0.4246(3) 0.5403(3) 0.6500(3) 0.0186(10) Uani 1 1 d . . . H6 H 0.4543 0.5566 0.6039 0.022 Uiso 1 1 calc R . . C7 C 0.3351(3) 0.4826(3) 0.7252(3) 0.0307(12) Uani 1 1 d . . . H7 H 0.2910 0.4503 0.7421 0.037 Uiso 1 1 calc R . . C8 C 0.3819(3) 0.5303(3) 0.7731(3) 0.0294(12) Uani 1 1 d . . . H8 H 0.3761 0.5378 0.8295 0.035 Uiso 1 1 calc R . . C9 C 0.5034(3) 0.6217(3) 0.7507(3) 0.0207(10) Uani 1 1 d . . . H9A H 0.5271 0.6030 0.8021 0.025 Uiso 1 1 calc R . . H9B H 0.4803 0.6759 0.7595 0.025 Uiso 1 1 calc R . . C10 C 0.5682(3) 0.6263(3) 0.6873(3) 0.0169(10) Uani 1 1 d . . . C11 C 0.6282(3) 0.5659(3) 0.6865(3) 0.0159(9) Uani 1 1 d . . . C12 C 0.6303(3) 0.5020(3) 0.7513(3) 0.0217(10) Uani 1 1 d . . . H12A H 0.6531 0.4516 0.7289 0.026 Uiso 1 1 calc R . . H12B H 0.5748 0.4905 0.7700 0.026 Uiso 1 1 calc R . . C13 C 0.6821(3) 0.5303(3) 0.8231(3) 0.0340(13) Uani 1 1 d . . . H13A H 0.7369 0.5417 0.8045 0.051 Uiso 1 1 calc R . . H13B H 0.6836 0.4879 0.8642 0.051 Uiso 1 1 calc R . . H13C H 0.6585 0.5792 0.8462 0.051 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 Br1 0.0474(3) 0.0474(3) 0.0474(3) 0.0122(3) 0.0122(3) 0.0122(3) Fe1 0.0229(3) 0.0229(3) 0.0229(3) 0.0008(3) 0.0008(3) 0.0008(3) Fe2 0.0407(4) 0.0407(4) 0.0407(4) -0.0074(4) 0.0074(4) -0.0074(4) Cl1 0.0316(7) 0.0313(7) 0.0273(7) 0.0074(5) 0.0046(6) 0.0066(6) Cl2 0.0356(6) 0.0356(6) 0.0356(6) -0.0139(5) -0.0139(5) -0.0139(5) Cl3 0.0629(8) 0.0629(8) 0.0629(8) 0.0178(7) -0.0178(7) 0.0178(7) Cl4 0.0268(8) 0.0395(9) 0.0928(13) -0.0299(9) 0.0043(8) -0.0033(6) N5 0.019(2) 0.0174(19) 0.017(2) 0.0020(16) 0.0034(17) -0.0039(16) N9 0.0154(19) 0.021(2) 0.014(2) -0.0019(16) 0.0035(16) -0.0012(16) C1 0.038(3) 0.023(3) 0.037(3) 0.003(3) 0.000(2) -0.008(2) C2 0.022(3) 0.022(3) 0.024(3) 0.006(2) -0.001(2) -0.001(2) C3 0.015(2) 0.017(2) 0.016(2) -0.0011(18) -0.0055(19) -0.0034(19) C4 0.011(2) 0.019(2) 0.018(2) -0.0043(19) -0.0047(19) -0.0074(19) C5 0.013(2) 0.031(3) 0.019(2) 0.002(2) 0.0007(19) 0.000(2) C6 0.019(2) 0.018(2) 0.019(3) 0.004(2) 0.0014(19) -0.001(2) C7 0.026(3) 0.040(3) 0.025(3) 0.001(2) 0.009(2) -0.012(2) C8 0.033(3) 0.037(3) 0.018(3) -0.002(2) 0.008(2) -0.007(2) C9 0.025(2) 0.020(2) 0.017(2) -0.001(2) -0.002(2) -0.0001(19) C10 0.015(2) 0.017(2) 0.019(2) -0.0052(19) -0.0003(18) -0.0023(19) C11 0.013(2) 0.019(2) 0.015(2) -0.0002(18) -0.0026(18) -0.0034(19) C12 0.021(2) 0.025(3) 0.019(3) 0.007(2) 0.004(2) 0.003(2) C13 0.036(3) 0.044(3) 0.021(3) 0.009(3) -0.001(2) 0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Cl2 2.190(2) . ? Fe1 Cl1 2.1952(13) 3 ? Fe1 Cl1 2.1952(13) 2 ? Fe1 Cl1 2.1952(13) . ? Fe2 Cl4 2.1967(15) . ? Fe2 Cl4 2.1967(15) 4_565 ? Fe2 Cl4 2.1967(15) 5_456 ? Fe2 Cl3 2.211(3) . ? N5 C6 1.333(6) . ? N5 C8 1.359(6) . ? N5 C9 1.494(6) . ? N9 C6 1.317(5) . ? N9 C7 1.349(6) . ? N9 C5 1.475(5) . ? C1 C2 1.498(6) . ? C2 C3 1.491(6) . ? C3 C4 1.398(6) 2 ? C3 C4 1.407(6) . ? C4 C3 1.398(6) 3 ? C4 C5 1.526(6) . ? C7 C8 1.364(6) . ? C9 C10 1.506(6) . ? C10 C11 1.402(6) 3 ? C10 C11 1.412(6) . ? C11 C10 1.402(6) 2 ? C11 C12 1.513(6) . ? C12 C13 1.543(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Fe1 Cl1 111.74(4) . 3 ? Cl2 Fe1 Cl1 111.74(4) . 2 ? Cl1 Fe1 Cl1 107.11(5) 3 2 ? Cl2 Fe1 Cl1 111.74(4) . . ? Cl1 Fe1 Cl1 107.11(5) 3 . ? Cl1 Fe1 Cl1 107.11(5) 2 . ? Cl4 Fe2 Cl4 110.83(6) . 4_565 ? Cl4 Fe2 Cl4 110.83(6) . 5_456 ? Cl4 Fe2 Cl4 110.83(6) 4_565 5_456 ? Cl4 Fe2 Cl3 108.07(6) . . ? Cl4 Fe2 Cl3 108.07(6) 4_565 . ? Cl4 Fe2 Cl3 108.07(6) 5_456 . ? C6 N5 C8 107.4(4) . . ? C6 N5 C9 125.8(4) . . ? C8 N5 C9 126.8(4) . . ? C6 N9 C7 108.6(4) . . ? C6 N9 C5 126.0(4) . . ? C7 N9 C5 125.4(4) . . ? C3 C2 C1 112.8(4) . . ? C4 C3 C4 118.6(5) 2 . ? C4 C3 C2 120.8(4) 2 . ? C4 C3 C2 120.7(4) . . ? C3 C4 C3 121.4(5) 3 . ? C3 C4 C5 119.1(4) 3 . ? C3 C4 C5 119.3(4) . . ? N9 C5 C4 110.1(3) . . ? N9 C6 N5 109.6(4) . . ? C8 C7 N9 107.1(4) . . ? C7 C8 N5 107.3(4) . . ? N5 C9 C10 110.5(3) . . ? C11 C10 C11 121.2(4) 3 . ? C11 C10 C9 120.4(4) 3 . ? C11 C10 C9 118.3(4) . . ? C10 C11 C10 118.8(4) 2 . ? C10 C11 C12 120.7(4) 2 . ? C10 C11 C12 120.5(4) . . ? C11 C12 C13 110.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.661 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.091 # Attachment '07srv231.cif' data_c:\rawdat~1\charlo~1\07srv231\work\k _database_code_depnum_ccdc_archive 'CCDC 650054' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H49 Ag N6, 2(F6 P)' _chemical_formula_sum 'C39 H49 Ag F12 N6 P2' _chemical_formula_weight 999.65 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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 12.4533(12) _cell_length_b 15.5863(15) _cell_length_c 22.8102(18) _cell_angle_alpha 90.00 _cell_angle_beta 112.441(4) _cell_angle_gamma 90.00 _cell_volume 4092.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.641796 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1k' _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 48483 _diffrn_reflns_av_R_equivalents 0.3042 _diffrn_reflns_av_sigmaI/netI 0.3135 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 29.18 _reflns_number_total 11030 _reflns_number_gt 4288 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics X-Seed _computing_publication_material X-Seed _refine_special_details ; A very small crystal was used and hence diffraction was weak meaning not many observable reflections. The Ag atom is disodered over two sites, this means the cage is also disordered but the data was not of suitable quality to be able to refine this. 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^+10.1864P] 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 calc _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11030 _refine_ls_number_parameters 557 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2866 _refine_ls_R_factor_gt 0.1216 _refine_ls_wR_factor_ref 0.2215 _refine_ls_wR_factor_gt 0.1720 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.11447(6) 0.76500(5) 0.42230(3) 0.0269(2) Uani 0.893(2) 1 d P A 1 Ag2 Ag 0.2571(6) 0.8056(5) 0.3570(3) 0.042(3) Uani 0.107(2) 1 d P A 2 P1 P 0.5752(3) 0.88366(19) 0.25789(12) 0.0504(8) Uani 1 1 d . . . P2 P -0.1172(2) 0.72199(18) 0.53881(12) 0.0438(7) Uani 1 1 d . . . F1 F 0.6041(6) 0.8656(4) 0.3303(3) 0.074(2) Uani 1 1 d . . . F2 F 0.5442(5) 0.9046(4) 0.1849(2) 0.0658(18) Uani 1 1 d . . . F3 F 0.5915(14) 0.7881(5) 0.2464(4) 0.200(6) Uani 1 1 d . . . F4 F 0.4467(8) 0.8712(9) 0.2449(3) 0.195(7) Uani 1 1 d . . . F5 F 0.5704(6) 0.9809(4) 0.2714(3) 0.079(2) Uani 1 1 d . . . F6 F 0.7068(6) 0.8962(6) 0.2696(3) 0.102(3) Uani 1 1 d . . . F7 F -0.1535(6) 0.7975(4) 0.5732(3) 0.080(2) Uani 1 1 d . . . F8 F -0.0810(5) 0.6432(4) 0.5053(3) 0.0579(16) Uani 1 1 d . . . F9 F -0.0776(5) 0.6679(4) 0.6033(2) 0.0557(16) Uani 1 1 d . . . F10 F 0.0080(5) 0.7606(4) 0.5599(3) 0.0694(18) Uani 1 1 d . . . F11 F -0.2440(5) 0.6796(4) 0.5187(3) 0.0648(18) Uani 1 1 d . . . F12 F -0.1582(6) 0.7735(4) 0.4750(3) 0.083(2) Uani 1 1 d . . . N1 N 0.2506(6) 0.6790(4) 0.5540(3) 0.0279(17) Uani 1 1 d . A . N2 N 0.1467(6) 0.5864(5) 0.4863(3) 0.0290(17) Uani 1 1 d . A . N3 N 0.0955(7) 0.9419(6) 0.3554(4) 0.046(2) Uani 1 1 d . A . N4 N -0.0097(7) 0.8492(5) 0.2896(4) 0.043(2) Uani 1 1 d . A . N5 N 0.4994(6) 0.7371(4) 0.4005(3) 0.0281(16) Uani 1 1 d . A . N6 N 0.3903(6) 0.6471(5) 0.3311(3) 0.0317(18) Uani 1 1 d . A . C1 C 0.1766(8) 0.6716(6) 0.4927(4) 0.035(2) Uani 1 1 d . . . C2 C 0.2673(8) 0.6017(6) 0.5855(4) 0.034(2) Uani 1 1 d . . . H2 H 0.3161 0.5913 0.6285 0.040 Uiso 1 1 calc R A . C3 C 0.2012(8) 0.5436(7) 0.5434(4) 0.040(2) Uani 1 1 d . A . H3 H 0.1934 0.4846 0.5513 0.049 Uiso 1 1 calc R . . C4 C 0.0664(8) 0.5448(6) 0.4276(4) 0.037(2) Uani 1 1 d . . . H4A H -0.0142 0.5498 0.4256 0.045 Uiso 1 1 calc R A . H4B H 0.0855 0.4830 0.4287 0.045 Uiso 1 1 calc R . . C5 C 0.0738(8) 0.5845(6) 0.3696(4) 0.036(2) Uani 1 1 d . A . C6 C -0.0100(8) 0.6473(6) 0.3346(4) 0.035(2) Uani 1 1 d . . . C7 C 0.0091(8) 0.6930(6) 0.2868(4) 0.038(2) Uani 1 1 d . A . C8 C 0.1036(8) 0.6761(6) 0.2697(4) 0.033(2) Uani 1 1 d . . . C9 C 0.1830(7) 0.6115(6) 0.3043(4) 0.031(2) Uani 1 1 d . A . C10 C 0.1696(7) 0.5671(5) 0.3540(4) 0.029(2) Uani 1 1 d . . . C11 C 0.2537(8) 0.4963(6) 0.3871(4) 0.044(3) Uani 1 1 d . A . H11A H 0.2763 0.4666 0.3551 0.053 Uiso 1 1 calc R . . H11B H 0.2122 0.4540 0.4032 0.053 Uiso 1 1 calc R . . C12 C 0.3657(8) 0.5232(6) 0.4428(4) 0.047(3) Uani 1 1 d . . . H12A H 0.4151 0.5564 0.4265 0.070 Uiso 1 1 calc R A . H12B H 0.4075 0.4718 0.4645 0.070 Uiso 1 1 calc R . . H12C H 0.3454 0.5584 0.4726 0.070 Uiso 1 1 calc R . . C13 C 0.2900(8) 0.5973(7) 0.2881(4) 0.045(3) Uani 1 1 d . . . H13A H 0.3098 0.5355 0.2918 0.054 Uiso 1 1 calc R A . H13B H 0.2723 0.6151 0.2437 0.054 Uiso 1 1 calc R . . C14 C 0.1128(8) 0.7197(7) 0.2128(5) 0.054(3) Uani 1 1 d . A . H14A H 0.0346 0.7400 0.1850 0.064 Uiso 1 1 calc R . . H14B H 0.1379 0.6767 0.1887 0.064 Uiso 1 1 calc R . . C15 C 0.1957(10) 0.7948(7) 0.2278(5) 0.068(4) Uani 1 1 d . . . H15A H 0.1774 0.8349 0.2558 0.102 Uiso 1 1 calc R A . H15B H 0.1879 0.8241 0.1884 0.102 Uiso 1 1 calc R . . H15C H 0.2755 0.7741 0.2491 0.102 Uiso 1 1 calc R . . C16 C -0.0687(8) 0.7699(7) 0.2585(4) 0.046(3) Uani 1 1 d . . . H16A H -0.0864 0.7731 0.2124 0.055 Uiso 1 1 calc R A . H16B H -0.1428 0.7635 0.2645 0.055 Uiso 1 1 calc R . . C17 C -0.1226(8) 0.6592(7) 0.3468(4) 0.051(3) Uani 1 1 d . A . H17A H -0.1063 0.6493 0.3922 0.062 Uiso 1 1 calc R . . H17B H -0.1508 0.7188 0.3363 0.062 Uiso 1 1 calc R . . C18 C -0.2147(9) 0.5978(9) 0.3072(5) 0.073(4) Uani 1 1 d . . . H18A H -0.2352 0.6105 0.2622 0.110 Uiso 1 1 calc R A . H18B H -0.2838 0.6038 0.3176 0.110 Uiso 1 1 calc R . . H18C H -0.1853 0.5389 0.3161 0.110 Uiso 1 1 calc R . . C19 C 0.3912(7) 0.7101(6) 0.3698(4) 0.032(2) Uani 1 1 d . . . H19 H 0.3246 0.7328 0.3750 0.039 Uiso 1 1 calc R A . C20 C 0.5030(8) 0.6335(6) 0.3362(4) 0.038(2) Uani 1 1 d . . . H20 H 0.5290 0.5919 0.3141 0.046 Uiso 1 1 calc R A . C21 C 0.5688(8) 0.6913(6) 0.3790(5) 0.040(2) Uani 1 1 d . A . H21 H 0.6503 0.6985 0.3918 0.048 Uiso 1 1 calc R . . C22 C 0.5363(7) 0.8094(5) 0.4464(4) 0.027(2) Uani 1 1 d . . . H22A H 0.5584 0.8591 0.4264 0.032 Uiso 1 1 calc R A . H22B H 0.6054 0.7920 0.4838 0.032 Uiso 1 1 calc R . . C23 C 0.4392(8) 0.8358(6) 0.4679(4) 0.032(2) Uani 1 1 d . A . C24 C 0.3615(8) 0.8998(6) 0.4342(4) 0.037(2) Uani 1 1 d . . . C25 C 0.2720(8) 0.9242(6) 0.4528(4) 0.036(2) Uani 1 1 d . A . C26 C 0.2579(8) 0.8839(5) 0.5048(4) 0.033(2) Uani 1 1 d . . . C27 C 0.3323(7) 0.8163(5) 0.5363(4) 0.028(2) Uani 1 1 d . A . C28 C 0.4261(8) 0.7931(5) 0.5186(4) 0.032(2) Uani 1 1 d . . . C29 C 0.5070(7) 0.7200(6) 0.5510(4) 0.034(2) Uani 1 1 d . A . H29A H 0.5346 0.6921 0.5204 0.041 Uiso 1 1 calc R . . H29B H 0.4640 0.6766 0.5652 0.041 Uiso 1 1 calc R . . C30 C 0.6108(8) 0.7513(6) 0.6078(4) 0.041(2) Uani 1 1 d . . . H30A H 0.6589 0.7887 0.5932 0.062 Uiso 1 1 calc R A . H30B H 0.6570 0.7019 0.6303 0.062 Uiso 1 1 calc R . . H30C H 0.5836 0.7833 0.6364 0.062 Uiso 1 1 calc R . . C31 C 0.3098(8) 0.7600(6) 0.5840(4) 0.040(2) Uani 1 1 d . . . H31A H 0.3844 0.7462 0.6189 0.048 Uiso 1 1 calc R A . H31B H 0.2606 0.7913 0.6022 0.048 Uiso 1 1 calc R . . C32 C 0.1616(8) 0.9117(6) 0.5267(4) 0.039(2) Uani 1 1 d . A . H32A H 0.0940 0.9316 0.4895 0.047 Uiso 1 1 calc R . . H32B H 0.1366 0.8616 0.5450 0.047 Uiso 1 1 calc R . . C33 C 0.1997(10) 0.9824(8) 0.5753(5) 0.072(4) Uani 1 1 d . . . H33A H 0.2648 0.9622 0.6129 0.109 Uiso 1 1 calc R A . H33B H 0.1348 0.9987 0.5873 0.109 Uiso 1 1 calc R . . H33C H 0.2244 1.0322 0.5574 0.109 Uiso 1 1 calc R . . C34 C 0.1778(9) 0.9855(6) 0.4111(5) 0.051(3) Uani 1 1 d . . . H34A H 0.1355 1.0099 0.4362 0.061 Uiso 1 1 calc R A . H34B H 0.2146 1.0335 0.3972 0.061 Uiso 1 1 calc R . . C35 C 0.3715(9) 0.9393(6) 0.3744(5) 0.047(3) Uani 1 1 d . A . H35A H 0.4040 0.8965 0.3537 0.056 Uiso 1 1 calc R . . H35B H 0.2934 0.9561 0.3439 0.056 Uiso 1 1 calc R . . C36 C 0.4482(9) 1.0160(6) 0.3925(5) 0.059(3) Uani 1 1 d . . . H36A H 0.4146 1.0589 0.4119 0.088 Uiso 1 1 calc R A . H36B H 0.4555 1.0403 0.3546 0.088 Uiso 1 1 calc R . . H36C H 0.5252 0.9992 0.4229 0.088 Uiso 1 1 calc R . . C37 C 0.0617(9) 0.8581(6) 0.3491(5) 0.041(2) Uani 1 1 d . . . C38 C -0.0238(9) 0.9221(8) 0.2559(6) 0.071(4) Uani 1 1 d . . . H38 H -0.0707 0.9299 0.2123 0.085 Uiso 1 1 calc R A . C39 C 0.0407(10) 0.9812(8) 0.2958(6) 0.066(4) Uani 1 1 d . A . H39 H 0.0486 1.0395 0.2858 0.080 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 0.0290(4) 0.0243(4) 0.0263(4) 0.0012(4) 0.0092(3) -0.0001(4) Ag2 0.024(4) 0.050(5) 0.050(5) 0.005(3) 0.012(3) 0.017(3) P1 0.074(2) 0.049(2) 0.0328(15) -0.0015(13) 0.0252(15) -0.0183(16) P2 0.0448(17) 0.0453(18) 0.0445(15) -0.0004(13) 0.0206(13) -0.0050(14) F1 0.135(6) 0.052(4) 0.040(3) 0.008(3) 0.040(4) -0.001(4) F2 0.079(5) 0.087(5) 0.028(3) -0.003(3) 0.017(3) -0.020(4) F3 0.49(2) 0.061(6) 0.139(8) -0.009(5) 0.227(12) -0.032(8) F4 0.093(7) 0.428(19) 0.058(5) -0.015(8) 0.022(5) -0.151(10) F5 0.131(6) 0.062(5) 0.063(4) 0.015(3) 0.059(4) 0.013(4) F6 0.064(5) 0.183(9) 0.068(5) 0.039(5) 0.034(4) 0.043(5) F7 0.092(5) 0.042(4) 0.132(6) -0.024(4) 0.072(5) -0.006(3) F8 0.073(4) 0.063(4) 0.053(4) -0.010(3) 0.042(3) -0.004(3) F9 0.067(4) 0.063(4) 0.033(3) -0.002(3) 0.015(3) -0.010(3) F10 0.068(4) 0.084(5) 0.067(4) -0.006(4) 0.037(3) -0.034(4) F11 0.037(4) 0.058(4) 0.083(4) 0.008(3) 0.004(3) -0.001(3) F12 0.112(6) 0.065(4) 0.061(4) 0.025(4) 0.020(4) -0.002(4) N1 0.038(5) 0.028(4) 0.024(4) -0.002(3) 0.019(4) -0.009(4) N2 0.024(4) 0.033(5) 0.030(4) -0.001(3) 0.010(3) 0.000(4) N3 0.031(5) 0.054(6) 0.050(6) 0.010(5) 0.012(4) 0.002(4) N4 0.024(5) 0.050(6) 0.052(6) 0.031(5) 0.011(4) 0.023(4) N5 0.025(4) 0.028(4) 0.031(4) 0.000(3) 0.011(3) 0.005(4) N6 0.022(4) 0.038(5) 0.038(4) -0.008(4) 0.015(3) 0.002(4) C1 0.038(6) 0.043(6) 0.022(5) 0.003(4) 0.009(4) 0.007(5) C2 0.032(6) 0.042(6) 0.028(5) 0.001(4) 0.013(4) -0.017(5) C3 0.036(6) 0.054(7) 0.029(5) 0.012(5) 0.010(5) -0.003(5) C4 0.039(6) 0.028(5) 0.031(5) -0.008(4) -0.003(4) -0.014(4) C5 0.031(6) 0.044(6) 0.032(5) -0.010(5) 0.010(5) -0.007(5) C6 0.029(6) 0.051(6) 0.015(4) -0.018(4) -0.003(4) 0.006(5) C7 0.029(6) 0.060(7) 0.021(5) 0.008(4) 0.003(4) 0.008(5) C8 0.032(6) 0.038(6) 0.030(5) 0.000(4) 0.013(4) 0.003(5) C9 0.019(5) 0.035(6) 0.038(5) -0.023(4) 0.011(4) -0.001(4) C10 0.027(5) 0.030(5) 0.024(5) 0.000(4) 0.001(4) 0.001(4) C11 0.024(6) 0.047(7) 0.049(6) -0.016(5) 0.000(5) -0.006(5) C12 0.025(6) 0.057(7) 0.045(6) 0.009(5) -0.001(5) 0.006(5) C13 0.026(6) 0.061(7) 0.041(6) -0.017(5) 0.006(5) -0.002(5) C14 0.034(6) 0.073(8) 0.053(6) 0.010(6) 0.016(5) -0.012(6) C15 0.069(9) 0.077(9) 0.077(8) 0.018(7) 0.047(7) -0.006(7) C16 0.041(6) 0.058(7) 0.034(5) 0.007(5) 0.007(4) 0.002(6) C17 0.034(6) 0.090(9) 0.039(6) -0.003(6) 0.025(5) 0.016(6) C18 0.039(7) 0.130(12) 0.065(8) -0.023(8) 0.034(6) -0.013(7) C19 0.014(5) 0.042(6) 0.036(5) -0.008(4) 0.004(4) 0.009(4) C20 0.024(6) 0.044(6) 0.057(6) -0.013(5) 0.026(5) 0.004(5) C21 0.023(5) 0.040(6) 0.063(7) -0.009(5) 0.024(5) -0.001(5) C22 0.027(5) 0.031(5) 0.018(4) 0.004(4) 0.003(4) 0.002(4) C23 0.031(6) 0.027(5) 0.040(5) -0.001(4) 0.015(5) -0.001(4) C24 0.044(6) 0.042(6) 0.030(5) -0.006(4) 0.020(5) -0.004(5) C25 0.045(6) 0.026(5) 0.041(6) 0.009(4) 0.021(5) 0.004(5) C26 0.038(6) 0.016(5) 0.048(6) -0.019(4) 0.018(5) -0.015(4) C27 0.027(5) 0.023(5) 0.032(5) -0.007(4) 0.009(4) -0.007(4) C28 0.031(5) 0.025(5) 0.028(5) 0.000(4) -0.001(4) -0.003(4) C29 0.036(6) 0.033(6) 0.035(5) 0.003(4) 0.015(4) 0.002(4) C30 0.044(6) 0.039(7) 0.035(5) 0.001(4) 0.008(4) 0.008(5) C31 0.050(6) 0.035(6) 0.036(5) -0.002(5) 0.018(5) -0.005(5) C32 0.029(6) 0.043(6) 0.046(6) -0.016(5) 0.015(5) -0.001(5) C33 0.069(9) 0.079(9) 0.085(9) -0.038(7) 0.047(8) -0.019(7) C34 0.064(8) 0.041(6) 0.065(7) 0.009(6) 0.043(7) 0.015(6) C35 0.043(7) 0.039(6) 0.065(7) -0.004(5) 0.029(6) -0.004(5) C36 0.046(7) 0.040(7) 0.082(8) -0.010(6) 0.015(6) -0.010(6) C37 0.036(6) 0.040(7) 0.045(6) 0.003(5) 0.013(5) 0.008(5) C38 0.040(8) 0.057(8) 0.085(9) 0.028(7) -0.011(6) 0.005(6) C39 0.043(8) 0.054(8) 0.083(9) 0.030(7) 0.003(7) -0.003(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 C1 2.085(9) . ? Ag1 C37 2.118(10) . ? P1 F4 1.524(8) . ? P1 F3 1.539(9) . ? P1 F5 1.552(7) . ? P1 F6 1.570(7) . ? P1 F1 1.575(6) . ? P1 F2 1.593(6) . ? P2 F10 1.566(6) . ? P2 F12 1.568(6) . ? P2 F7 1.574(6) . ? P2 F8 1.599(6) . ? P2 F9 1.601(6) . ? P2 F11 1.608(6) . ? N1 C1 1.356(10) . ? N1 C2 1.376(10) . ? N1 C31 1.491(10) . ? N2 C1 1.371(11) . ? N2 C3 1.389(10) . ? N2 C4 1.481(10) . ? N3 C37 1.364(12) . ? N3 C39 1.408(12) . ? N3 C34 1.460(13) . ? N4 C37 1.316(11) . ? N4 C38 1.345(12) . ? N4 C16 1.474(12) . ? N5 C19 1.327(10) . ? N5 C21 1.350(10) . ? N5 C22 1.487(10) . ? N6 C19 1.318(10) . ? N6 C20 1.380(10) . ? N6 C13 1.480(11) . ? C2 C3 1.347(12) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.494(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.396(12) . ? C5 C6 1.431(12) . ? C6 C7 1.397(12) . ? C6 C17 1.541(12) . ? C7 C8 1.398(12) . ? C7 C16 1.522(13) . ? C8 C9 1.420(12) . ? C8 C14 1.507(12) . ? C9 C10 1.393(12) . ? C9 C13 1.529(11) . ? C10 C11 1.511(12) . ? C11 C12 1.543(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.511(14) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.502(14) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19 0.9500 . ? C20 C21 1.351(12) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.524(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C28 1.396(11) . ? C23 C24 1.399(12) . ? C24 C25 1.389(12) . ? C24 C35 1.543(12) . ? C25 C26 1.411(11) . ? C25 C34 1.531(13) . ? C26 C27 1.406(12) . ? C26 C32 1.526(12) . ? C27 C28 1.421(12) . ? C27 C31 1.503(11) . ? C28 C29 1.514(11) . ? C29 C30 1.519(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.506(12) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.486(12) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C38 C39 1.327(15) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? 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 C37 176.0(4) . . ? F4 P1 F3 92.4(8) . . ? F4 P1 F5 92.6(7) . . ? F3 P1 F5 175.0(7) . . ? F4 P1 F6 178.6(4) . . ? F3 P1 F6 87.2(7) . . ? F5 P1 F6 87.8(4) . . ? F4 P1 F1 89.2(4) . . ? F3 P1 F1 90.8(4) . . ? F5 P1 F1 88.7(3) . . ? F6 P1 F1 92.1(4) . . ? F4 P1 F2 90.3(4) . . ? F3 P1 F2 90.8(4) . . ? F5 P1 F2 89.7(3) . . ? F6 P1 F2 88.4(3) . . ? F1 P1 F2 178.3(4) . . ? F10 P2 F12 91.2(4) . . ? F10 P2 F7 90.1(4) . . ? F12 P2 F7 91.5(4) . . ? F10 P2 F8 90.7(3) . . ? F12 P2 F8 90.0(3) . . ? F7 P2 F8 178.2(4) . . ? F10 P2 F9 89.9(3) . . ? F12 P2 F9 178.7(4) . . ? F7 P2 F9 89.0(3) . . ? F8 P2 F9 89.5(3) . . ? F10 P2 F11 178.1(4) . . ? F12 P2 F11 90.5(4) . . ? F7 P2 F11 90.7(3) . . ? F8 P2 F11 88.5(3) . . ? F9 P2 F11 88.3(3) . . ? C1 N1 C2 111.8(7) . . ? C1 N1 C31 124.6(7) . . ? C2 N1 C31 123.6(7) . . ? C1 N2 C3 110.5(7) . . ? C1 N2 C4 125.7(7) . . ? C3 N2 C4 123.9(8) . . ? C37 N3 C39 107.4(9) . . ? C37 N3 C34 128.6(8) . . ? C39 N3 C34 124.0(9) . . ? C37 N4 C38 112.9(10) . . ? C37 N4 C16 127.0(8) . . ? C38 N4 C16 120.1(9) . . ? C19 N5 C21 107.6(7) . . ? C19 N5 C22 126.2(7) . . ? C21 N5 C22 126.0(7) . . ? C19 N6 C20 108.0(7) . . ? C19 N6 C13 128.7(7) . . ? C20 N6 C13 123.3(7) . . ? N1 C1 N2 104.0(7) . . ? N1 C1 Ag1 129.9(7) . . ? N2 C1 Ag1 126.0(6) . . ? C3 C2 N1 106.7(8) . . ? C3 C2 H2 126.7 . . ? N1 C2 H2 126.7 . . ? C2 C3 N2 107.0(8) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? N2 C4 C5 111.7(7) . . ? N2 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C10 C5 C6 120.1(8) . . ? C10 C5 C4 119.5(9) . . ? C6 C5 C4 120.0(8) . . ? C7 C6 C5 118.7(8) . . ? C7 C6 C17 121.2(8) . . ? C5 C6 C17 120.0(9) . . ? C6 C7 C8 122.2(8) . . ? C6 C7 C16 117.5(8) . . ? C8 C7 C16 119.8(8) . . ? C7 C8 C9 117.4(8) . . ? C7 C8 C14 120.2(8) . . ? C9 C8 C14 122.1(8) . . ? C10 C9 C8 122.0(8) . . ? C10 C9 C13 120.8(8) . . ? C8 C9 C13 117.1(8) . . ? C9 C10 C5 119.4(8) . . ? C9 C10 C11 119.6(8) . . ? C5 C10 C11 120.8(8) . . ? C10 C11 C12 116.7(8) . . ? C10 C11 H11A 108.1 . . ? C12 C11 H11A 108.1 . . ? C10 C11 H11B 108.1 . . ? C12 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N6 C13 C9 110.9(7) . . ? N6 C13 H13A 109.5 . . ? C9 C13 H13A 109.5 . . ? N6 C13 H13B 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 108.0 . . ? C8 C14 C15 115.1(8) . . ? C8 C14 H14A 108.5 . . ? C15 C14 H14A 108.5 . . ? C8 C14 H14B 108.5 . . ? C15 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? 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 . . ? N4 C16 C7 109.7(7) . . ? N4 C16 H16A 109.7 . . ? C7 C16 H16A 109.7 . . ? N4 C16 H16B 109.7 . . ? C7 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C18 C17 C6 110.7(8) . . ? C18 C17 H17A 109.5 . . ? C6 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C6 C17 H17B 109.5 . . ? H17A C17 H17B 108.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 N5 109.7(7) . . ? N6 C19 H19 125.1 . . ? N5 C19 H19 125.1 . . ? C21 C20 N6 105.9(8) . . ? C21 C20 H20 127.0 . . ? N6 C20 H20 127.0 . . ? N5 C21 C20 108.7(8) . . ? N5 C21 H21 125.7 . . ? C20 C21 H21 125.7 . . ? N5 C22 C23 111.1(7) . . ? N5 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? N5 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C28 C23 C24 121.3(8) . . ? C28 C23 C22 119.7(8) . . ? C24 C23 C22 118.8(8) . . ? C25 C24 C23 119.6(8) . . ? C25 C24 C35 120.4(9) . . ? C23 C24 C35 119.9(8) . . ? C24 C25 C26 120.5(8) . . ? C24 C25 C34 119.7(8) . . ? C26 C25 C34 119.2(8) . . ? C27 C26 C25 119.6(8) . . ? C27 C26 C32 119.5(8) . . ? C25 C26 C32 120.9(8) . . ? C26 C27 C28 119.8(8) . . ? C26 C27 C31 122.6(8) . . ? C28 C27 C31 117.3(8) . . ? C23 C28 C27 118.9(8) . . ? C23 C28 C29 119.8(8) . . ? C27 C28 C29 121.2(8) . . ? C28 C29 C30 111.5(7) . . ? C28 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? C28 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C31 C27 111.1(7) . . ? N1 C31 H31A 109.4 . . ? C27 C31 H31A 109.4 . . ? N1 C31 H31B 109.4 . . ? C27 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C33 C32 C26 112.5(8) . . ? C33 C32 H32A 109.1 . . ? C26 C32 H32A 109.1 . . ? C33 C32 H32B 109.1 . . ? C26 C32 H32B 109.1 . . ? H32A C32 H32B 107.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 C25 111.5(8) . . ? N3 C34 H34A 109.3 . . ? C25 C34 H34A 109.3 . . ? N3 C34 H34B 109.3 . . ? C25 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C24 109.6(8) . . ? C36 C35 H35A 109.7 . . ? C24 C35 H35A 109.7 . . ? C36 C35 H35B 109.7 . . ? C24 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 N3 105.6(8) . . ? N4 C37 Ag1 128.7(8) . . ? N3 C37 Ag1 125.7(7) . . ? C39 C38 N4 106.4(10) . . ? C39 C38 H38 126.8 . . ? N4 C38 H38 126.8 . . ? C38 C39 N3 107.7(10) . . ? C38 C39 H39 126.2 . . ? N3 C39 H39 126.2 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.723 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.123