# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Sylvie Ferlay' _publ_contact_author_email ferlay@unistra.fr _publ_author_name M.W.Hosseini data_e940a _database_code_depnum_ccdc_archive 'CCDC 790491' #TrackingRef '1D Ag(CN)2 C3 (940).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H44 N4, 2(C2 Ag N2)' _chemical_formula_sum 'C30 H44 Ag2 N8' _chemical_formula_weight 732.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.7993(4) _cell_length_b 19.1350(10) _cell_length_c 12.7204(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.261(2) _cell_angle_gamma 90.00 _cell_volume 1650.41(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2699 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 27.35 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 1.218 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7928 _exptl_absorpt_correction_T_max 0.9416 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 9385 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3700 _reflns_number_gt 2394 _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^)+(0.0083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3700 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0540 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.004 _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 C1 C 0.8218(4) 0.42388(14) 0.42055(18) 0.0229(7) Uani 1 1 d . . . N1 N 0.9679(3) 0.40280(12) 0.48729(15) 0.0270(6) Uani 1 1 d . . . H3 H 0.9656 0.4142 0.5542 0.032 Uiso 1 1 calc R . . C2 C 1.1318(4) 0.36164(16) 0.45506(18) 0.0293(7) Uani 1 1 d . . . H7A H 1.1740 0.3286 0.5122 0.035 Uiso 1 1 calc R . . H7B H 1.2441 0.3931 0.4442 0.035 Uiso 1 1 calc R . . C3 C 1.0795(4) 0.32050(15) 0.35335(19) 0.0264(7) Uani 1 1 d . . . C4 C 0.9867(4) 0.37386(16) 0.27396(19) 0.0287(7) Uani 1 1 d . . . H8A H 1.0878 0.4081 0.2555 0.034 Uiso 1 1 calc R . . H8B H 0.9372 0.3495 0.2086 0.034 Uiso 1 1 calc R . . N2 N 0.8238(3) 0.41046(12) 0.31920(15) 0.0284(6) Uani 1 1 d . . . H4 H 0.7229 0.4241 0.2768 0.034 Uiso 1 1 calc R . . C5 C 0.9248(5) 0.26298(17) 0.3678(2) 0.0418(8) Uani 1 1 d . . . H13A H 0.7948 0.2863 0.3672 0.050 Uiso 1 1 calc R . . H13B H 0.9213 0.2328 0.3044 0.050 Uiso 1 1 calc R . . C6 C 0.9416(6) 0.2169(2) 0.4596(3) 0.0663(12) Uani 1 1 d . . . H14A H 0.9402 0.2457 0.5241 0.080 Uiso 1 1 calc R . . H14B H 1.0704 0.1926 0.4617 0.080 Uiso 1 1 calc R . . C7 C 0.7791(5) 0.1625(2) 0.4609(2) 0.0602(11) Uani 1 1 d . . . H15A H 0.6536 0.1857 0.4713 0.090 Uiso 1 1 calc R . . H15B H 0.8103 0.1295 0.5186 0.090 Uiso 1 1 calc R . . H15C H 0.7687 0.1373 0.3937 0.090 Uiso 1 1 calc R . . C8 C 1.2740(4) 0.29229(16) 0.31544(19) 0.0321(7) Uani 1 1 d . . . H10A H 1.3693 0.3315 0.3164 0.038 Uiso 1 1 calc R . . H10B H 1.3273 0.2574 0.3675 0.038 Uiso 1 1 calc R . . C9 C 1.2670(4) 0.25875(16) 0.2070(2) 0.0357(8) Uani 1 1 d . . . H11A H 1.1717 0.2196 0.2042 0.043 Uiso 1 1 calc R . . H11B H 1.2200 0.2936 0.1533 0.043 Uiso 1 1 calc R . . C10 C 1.4676(4) 0.23161(19) 0.1810(2) 0.0504(10) Uani 1 1 d . . . H12A H 1.5627 0.2702 0.1843 0.076 Uiso 1 1 calc R . . H12B H 1.4577 0.2116 0.1098 0.076 Uiso 1 1 calc R . . H12C H 1.5118 0.1955 0.2320 0.076 Uiso 1 1 calc R . . C11 C 0.6562(4) 0.46308(14) 0.46117(19) 0.0230(7) Uani 1 1 d . . . C12 C 0.5496(4) 0.51156(15) 0.39771(19) 0.0246(7) Uani 1 1 d . . . H4A H 0.5835 0.5194 0.3276 0.030 Uiso 1 1 calc R . . C13 C 0.3963(4) 0.54790(15) 0.43600(18) 0.0244(7) Uani 1 1 d . . . H3A H 0.3252 0.5809 0.3922 0.029 Uiso 1 1 calc R . . Ag1 Ag 0.24997(3) 0.441414(15) 0.941338(16) 0.04259(9) Uani 1 1 d . . . C14 C 0.1033(4) 0.43212(18) 0.7939(2) 0.0383(8) Uani 1 1 d . . . N3 N 0.0304(3) 0.42406(14) 0.71077(17) 0.0414(7) Uani 1 1 d . . . C15 C 0.3996(4) 0.43757(17) 1.0889(2) 0.0361(8) Uani 1 1 d . . . N4 N 0.4961(3) 0.43396(14) 1.16582(16) 0.0386(7) 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 C1 0.0232(14) 0.0243(19) 0.0207(13) -0.0005(12) -0.0030(11) 0.0001(12) N1 0.0258(13) 0.0373(16) 0.0172(11) -0.0072(11) -0.0043(9) 0.0073(12) C2 0.0257(16) 0.039(2) 0.0225(14) -0.0066(13) -0.0056(11) 0.0048(14) C3 0.0266(16) 0.0318(19) 0.0202(13) -0.0043(13) -0.0027(11) 0.0016(14) C4 0.0255(16) 0.041(2) 0.0197(13) -0.0042(13) 0.0022(11) 0.0053(14) N2 0.0254(13) 0.0410(17) 0.0181(11) -0.0026(11) -0.0041(9) 0.0098(11) C5 0.052(2) 0.039(2) 0.0346(17) -0.0060(16) 0.0025(15) -0.0056(17) C6 0.084(3) 0.065(3) 0.048(2) 0.002(2) -0.0080(19) -0.021(2) C7 0.060(3) 0.068(3) 0.053(2) 0.015(2) 0.0058(17) -0.021(2) C8 0.0285(16) 0.041(2) 0.0263(14) -0.0080(14) -0.0035(12) 0.0084(15) C9 0.0325(18) 0.043(2) 0.0316(17) -0.0107(15) -0.0004(13) 0.0020(15) C10 0.038(2) 0.069(3) 0.044(2) -0.0242(18) -0.0023(15) 0.0136(18) C11 0.0196(14) 0.0262(19) 0.0228(13) -0.0027(12) -0.0020(11) 0.0000(12) C12 0.0247(15) 0.0335(19) 0.0157(12) 0.0009(12) 0.0009(11) 0.0000(14) C13 0.0245(14) 0.0270(19) 0.0207(13) 0.0013(13) -0.0046(10) 0.0015(14) Ag1 0.04597(15) 0.05773(19) 0.02184(11) 0.00282(13) -0.01230(9) -0.00687(15) C14 0.0380(18) 0.050(2) 0.0268(15) 0.0050(16) -0.0010(12) -0.0050(17) N3 0.0392(15) 0.059(2) 0.0249(13) -0.0036(13) -0.0055(11) 0.0010(13) C15 0.0361(17) 0.044(2) 0.0278(14) 0.0021(16) -0.0028(12) -0.0051(17) N4 0.0390(15) 0.051(2) 0.0241(12) -0.0009(13) -0.0067(10) 0.0039(14) _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 C1 N2 1.316(3) . ? C1 N1 1.321(3) . ? C1 C11 1.478(4) . ? N1 C2 1.448(3) . ? N1 H3 0.8800 . ? C2 C3 1.534(3) . ? C2 H7A 0.9900 . ? C2 H7B 0.9900 . ? C3 C4 1.538(3) . ? C3 C8 1.539(3) . ? C3 C5 1.543(4) . ? C4 N2 1.464(3) . ? C4 H8A 0.9900 . ? C4 H8B 0.9900 . ? N2 H4 0.8800 . ? C5 C6 1.461(4) . ? C5 H13A 0.9900 . ? C5 H13B 0.9900 . ? C6 C7 1.518(4) . ? C6 H14A 0.9900 . ? C6 H14B 0.9900 . ? C7 H15A 0.9800 . ? C7 H15B 0.9800 . ? C7 H15C 0.9800 . ? C8 C9 1.519(3) . ? C8 H10A 0.9900 . ? C8 H10B 0.9900 . ? C9 C10 1.518(4) . ? C9 H11A 0.9900 . ? C9 H11B 0.9900 . ? C10 H12A 0.9800 . ? C10 H12B 0.9800 . ? C10 H12C 0.9800 . ? C11 C12 1.397(3) . ? C11 C13 1.397(3) 3_666 ? C12 C13 1.372(3) . ? C12 H4A 0.9500 . ? C13 C11 1.397(3) 3_666 ? C13 H3A 0.9500 . ? Ag1 C14 2.066(3) . ? Ag1 C15 2.069(2) . ? C14 N3 1.144(3) . ? C15 N4 1.139(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 120.6(2) . . ? N2 C1 C11 120.3(2) . . ? N1 C1 C11 119.1(2) . . ? C1 N1 C2 122.8(2) . . ? C1 N1 H3 118.6 . . ? C2 N1 H3 118.6 . . ? N1 C2 C3 112.5(2) . . ? N1 C2 H7A 109.1 . . ? C3 C2 H7A 109.1 . . ? N1 C2 H7B 109.1 . . ? C3 C2 H7B 109.1 . . ? H7A C2 H7B 107.8 . . ? C2 C3 C4 105.7(2) . . ? C2 C3 C8 107.1(2) . . ? C4 C3 C8 110.3(2) . . ? C2 C3 C5 112.5(2) . . ? C4 C3 C5 107.6(2) . . ? C8 C3 C5 113.4(3) . . ? N2 C4 C3 110.2(2) . . ? N2 C4 H8A 109.6 . . ? C3 C4 H8A 109.6 . . ? N2 C4 H8B 109.6 . . ? C3 C4 H8B 109.6 . . ? H8A C4 H8B 108.1 . . ? C1 N2 C4 122.8(2) . . ? C1 N2 H4 118.6 . . ? C4 N2 H4 118.6 . . ? C6 C5 C3 120.9(2) . . ? C6 C5 H13A 107.1 . . ? C3 C5 H13A 107.1 . . ? C6 C5 H13B 107.1 . . ? C3 C5 H13B 107.1 . . ? H13A C5 H13B 106.8 . . ? C5 C6 C7 114.1(3) . . ? C5 C6 H14A 108.7 . . ? C7 C6 H14A 108.7 . . ? C5 C6 H14B 108.7 . . ? C7 C6 H14B 108.7 . . ? H14A C6 H14B 107.6 . . ? C6 C7 H15A 109.5 . . ? C6 C7 H15B 109.5 . . ? H15A C7 H15B 109.5 . . ? C6 C7 H15C 109.5 . . ? H15A C7 H15C 109.5 . . ? H15B C7 H15C 109.5 . . ? C9 C8 C3 117.6(2) . . ? C9 C8 H10A 107.9 . . ? C3 C8 H10A 107.9 . . ? C9 C8 H10B 107.9 . . ? C3 C8 H10B 107.9 . . ? H10A C8 H10B 107.2 . . ? C10 C9 C8 112.0(2) . . ? C10 C9 H11A 109.2 . . ? C8 C9 H11A 109.2 . . ? C10 C9 H11B 109.2 . . ? C8 C9 H11B 109.2 . . ? H11A C9 H11B 107.9 . . ? C9 C10 H12A 109.5 . . ? C9 C10 H12B 109.5 . . ? H12A C10 H12B 109.5 . . ? C9 C10 H12C 109.5 . . ? H12A C10 H12C 109.5 . . ? H12B C10 H12C 109.5 . . ? C12 C11 C13 118.9(2) . 3_666 ? C12 C11 C1 120.7(2) . . ? C13 C11 C1 120.4(2) 3_666 . ? C13 C12 C11 120.5(2) . . ? C13 C12 H4A 119.8 . . ? C11 C12 H4A 119.8 . . ? C12 C13 C11 120.7(2) . 3_666 ? C12 C13 H3A 119.7 . . ? C11 C13 H3A 119.7 3_666 . ? C14 Ag1 C15 173.01(13) . . ? N3 C14 Ag1 175.9(3) . . ? N4 C15 Ag1 174.1(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.989 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.075 # Attachment '1D Ag(CN)2 C6 (393).cif' data_e393b _database_code_depnum_ccdc_archive 'CCDC 790492' #TrackingRef '1D Ag(CN)2 C6 (393).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C38 H68 N4, 2(C2 Ag N2)' _chemical_formula_sum 'C42 H68 Ag2 N8' _chemical_formula_weight 900.78 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' N N 0.0061 0.0033 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.4924(4) _cell_length_b 13.0691(8) _cell_length_c 13.8015(7) _cell_angle_alpha 90.224(2) _cell_angle_beta 95.777(2) _cell_angle_gamma 98.978(2) _cell_volume 1150.60(12) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2870 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 24.36 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_absorpt_coefficient_mu 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9654 _exptl_absorpt_correction_T_max 0.9739 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 9194 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5244 _reflns_number_gt 3968 _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^)+(0.0520P)^2^+0.0252P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5244 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 C1 C -0.1451(4) 0.09914(19) 0.40762(17) 0.0237(5) Uani 1 1 d . . . N1 N -0.0342(3) 0.04252(16) 0.36044(15) 0.0259(5) Uani 1 1 d . . . H1 H -0.0671 -0.0254 0.3606 0.031 Uiso 1 1 calc R . . C2 C 0.1415(4) 0.0886(2) 0.3078(2) 0.0286(6) Uani 1 1 d . . . H2A H 0.1491 0.0444 0.2502 0.034 Uiso 1 1 calc R . . H2B H 0.2741 0.0911 0.3506 0.034 Uiso 1 1 calc R . . C3 C 0.1178(4) 0.19838(19) 0.27448(18) 0.0245(5) Uani 1 1 d . . . C4 C 0.0779(4) 0.2571(2) 0.36584(19) 0.0264(5) Uani 1 1 d . . . H4A H 0.2047 0.2653 0.4132 0.032 Uiso 1 1 calc R . . H4B H 0.0483 0.3269 0.3478 0.032 Uiso 1 1 calc R . . N2 N -0.0998(3) 0.20028(16) 0.41039(15) 0.0252(5) Uani 1 1 d . . . H2 H -0.1799 0.2358 0.4404 0.030 Uiso 1 1 calc R . . C5 C -0.0692(4) 0.1981(2) 0.19605(18) 0.0257(5) Uani 1 1 d . . . H5A H -0.1989 0.1705 0.2255 0.031 Uiso 1 1 calc R . . H5B H -0.0778 0.2709 0.1788 0.031 Uiso 1 1 calc R . . C6 C -0.0672(5) 0.1368(2) 0.1022(2) 0.0374(7) Uani 1 1 d . . . H6A H 0.0654 0.1604 0.0735 0.045 Uiso 1 1 calc R . . H6B H -0.0731 0.0625 0.1171 0.045 Uiso 1 1 calc R . . C7 C -0.2512(5) 0.1502(2) 0.0285(2) 0.0384(7) Uani 1 1 d . . . H7A H -0.2417 0.2244 0.0121 0.046 Uiso 1 1 calc R . . H7B H -0.3832 0.1297 0.0587 0.046 Uiso 1 1 calc R . . C8 C -0.2600(5) 0.0866(3) -0.0651(2) 0.0516(8) Uani 1 1 d . . . H8A H -0.2796 0.0122 -0.0492 0.062 Uiso 1 1 calc R . . H8B H -0.1241 0.1035 -0.0927 0.062 Uiso 1 1 calc R . . C9 C -0.4376(7) 0.1056(3) -0.1431(3) 0.0645(11) Uani 1 1 d . . . H9A H -0.4617 0.0493 -0.1930 0.077 Uiso 1 1 calc R . . H9B H -0.5690 0.1052 -0.1123 0.077 Uiso 1 1 calc R . . C10 C -0.3806(7) 0.2076(4) -0.1904(3) 0.0768(13) Uani 1 1 d . . . H10A H -0.3616 0.2634 -0.1412 0.115 Uiso 1 1 calc R . . H10B H -0.4929 0.2180 -0.2406 0.115 Uiso 1 1 calc R . . H10C H -0.2499 0.2080 -0.2203 0.115 Uiso 1 1 calc R . . C11 C 0.3283(4) 0.2477(2) 0.23994(19) 0.0281(6) Uani 1 1 d . . . H11A H 0.4405 0.2429 0.2931 0.034 Uiso 1 1 calc R . . H11B H 0.3560 0.2061 0.1840 0.034 Uiso 1 1 calc R . . C12 C 0.3444(4) 0.3608(2) 0.2096(2) 0.0341(6) Uani 1 1 d . . . H12A H 0.2337 0.3668 0.1561 0.041 Uiso 1 1 calc R . . H12B H 0.3204 0.4037 0.2654 0.041 Uiso 1 1 calc R . . C13 C 0.5573(4) 0.4017(2) 0.1760(2) 0.0357(7) Uani 1 1 d . . . H13A H 0.6675 0.3935 0.2292 0.043 Uiso 1 1 calc R . . H13B H 0.5794 0.3590 0.1197 0.043 Uiso 1 1 calc R . . C14 C 0.5825(5) 0.5142(2) 0.1470(2) 0.0421(7) Uani 1 1 d . . . H14A H 0.5631 0.5572 0.2036 0.051 Uiso 1 1 calc R . . H14B H 0.4713 0.5228 0.0944 0.051 Uiso 1 1 calc R . . C15 C 0.7954(6) 0.5535(3) 0.1120(3) 0.0618(10) Uani 1 1 d . . . H15A H 0.9066 0.5473 0.1653 0.074 Uiso 1 1 calc R . . H15B H 0.8169 0.5093 0.0567 0.074 Uiso 1 1 calc R . . C16 C 0.8159(7) 0.6648(4) 0.0804(3) 0.0868(16) Uani 1 1 d . . . H16A H 0.7053 0.6717 0.0282 0.130 Uiso 1 1 calc R . . H16B H 0.9533 0.6854 0.0566 0.130 Uiso 1 1 calc R . . H16C H 0.8026 0.7094 0.1359 0.130 Uiso 1 1 calc R . . C17 C -0.3270(4) 0.04760(19) 0.45550(18) 0.0229(5) Uani 1 1 d . . . C18 C -0.4344(4) -0.0488(2) 0.42196(18) 0.0241(5) Uani 1 1 d . . . H18 H -0.3897 -0.0820 0.3683 0.029 Uiso 1 1 calc R . . C19 C -0.3952(4) 0.09642(19) 0.53410(18) 0.0246(5) Uani 1 1 d . . . H19 H -0.3241 0.1624 0.5572 0.029 Uiso 1 1 calc R . . Ag1 Ag 0.21934(4) 0.413490(17) 0.592162(17) 0.04461(11) Uani 1 1 d . . . C20 C 0.1320(5) 0.2629(2) 0.6336(2) 0.0378(7) Uani 1 1 d . . . N3 N 0.0826(4) 0.17866(19) 0.6529(2) 0.0407(6) Uani 1 1 d . . . C21 C 0.3005(5) 0.5649(2) 0.5538(2) 0.0403(7) Uani 1 1 d . . . N4 N 0.3427(4) 0.6500(2) 0.5349(2) 0.0460(7) 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 C1 0.0236(12) 0.0243(13) 0.0217(12) 0.0060(10) -0.0044(10) 0.0032(10) N1 0.0235(11) 0.0208(11) 0.0340(12) 0.0044(9) 0.0031(9) 0.0050(8) C2 0.0241(13) 0.0302(14) 0.0325(14) 0.0065(11) 0.0028(11) 0.0074(11) C3 0.0231(13) 0.0242(13) 0.0263(13) 0.0016(10) 0.0004(10) 0.0052(10) C4 0.0264(13) 0.0243(13) 0.0276(13) 0.0024(10) 0.0051(11) -0.0001(10) N2 0.0249(11) 0.0251(11) 0.0256(11) 0.0009(9) 0.0048(9) 0.0025(9) C5 0.0243(13) 0.0289(13) 0.0257(13) 0.0033(10) 0.0025(10) 0.0101(10) C6 0.0368(16) 0.0421(17) 0.0350(15) -0.0024(13) -0.0037(12) 0.0164(13) C7 0.0381(16) 0.0479(18) 0.0305(15) -0.0036(13) -0.0041(12) 0.0154(13) C8 0.054(2) 0.058(2) 0.0443(18) -0.0084(16) -0.0058(15) 0.0203(17) C9 0.087(3) 0.073(3) 0.0345(19) -0.0129(18) -0.0147(18) 0.032(2) C10 0.077(3) 0.088(3) 0.061(3) -0.008(2) -0.018(2) 0.016(3) C11 0.0230(13) 0.0309(14) 0.0309(14) 0.0040(11) 0.0038(11) 0.0047(11) C12 0.0298(14) 0.0336(15) 0.0400(16) 0.0081(12) 0.0089(12) 0.0043(12) C13 0.0302(14) 0.0386(16) 0.0389(16) 0.0050(13) 0.0104(13) 0.0026(12) C14 0.0392(16) 0.0438(18) 0.0408(17) 0.0084(14) 0.0067(14) -0.0033(14) C15 0.054(2) 0.065(2) 0.060(2) 0.0109(19) 0.0142(19) -0.0154(19) C16 0.086(3) 0.091(3) 0.069(3) 0.025(2) 0.010(2) -0.035(3) C17 0.0201(12) 0.0246(13) 0.0234(12) 0.0050(10) -0.0031(10) 0.0048(10) C18 0.0235(12) 0.0262(13) 0.0228(12) 0.0031(10) 0.0001(10) 0.0055(10) C19 0.0229(12) 0.0204(12) 0.0281(13) 0.0011(10) -0.0052(10) 0.0013(10) Ag1 0.06191(19) 0.02507(13) 0.04392(16) 0.00043(9) -0.00295(11) 0.00312(10) C20 0.0383(16) 0.0299(16) 0.0426(17) -0.0028(13) -0.0070(13) 0.0049(12) N3 0.0359(13) 0.0310(14) 0.0546(16) 0.0014(12) -0.0016(12) 0.0073(11) C21 0.0469(18) 0.0297(16) 0.0462(18) -0.0015(13) 0.0060(14) 0.0118(13) N4 0.0535(16) 0.0317(15) 0.0558(17) 0.0021(12) 0.0102(14) 0.0134(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 C1 N2 1.308(3) . ? C1 N1 1.322(3) . ? C1 C17 1.482(3) . ? N1 C2 1.465(3) . ? N1 H1 0.8800 . ? C2 C3 1.535(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.538(3) . ? C3 C11 1.539(3) . ? C3 C5 1.543(3) . ? C4 N2 1.463(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.523(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.521(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.525(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.547(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.496(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.528(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.514(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.524(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.509(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.394(3) . ? C17 C19 1.400(4) . ? C18 C19 1.379(4) 2_456 ? C18 H18 0.9500 . ? C19 C18 1.379(4) 2_456 ? C19 H19 0.9500 . ? Ag1 C21 2.053(3) . ? Ag1 C20 2.061(3) . ? C20 N3 1.138(4) . ? C21 N4 1.140(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 120.8(2) . . ? N2 C1 C17 119.5(2) . . ? N1 C1 C17 119.6(2) . . ? C1 N1 C2 122.5(2) . . ? C1 N1 H1 118.8 . . ? C2 N1 H1 118.8 . . ? N1 C2 C3 111.6(2) . . ? N1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 105.7(2) . . ? C2 C3 C11 107.3(2) . . ? C4 C3 C11 109.4(2) . . ? C2 C3 C5 111.9(2) . . ? C4 C3 C5 109.2(2) . . ? C11 C3 C5 113.0(2) . . ? N2 C4 C3 110.2(2) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 123.0(2) . . ? C1 N2 H2 118.5 . . ? C4 N2 H2 118.5 . . ? C6 C5 C3 117.3(2) . . ? C6 C5 H5A 108.0 . . ? C3 C5 H5A 108.0 . . ? C6 C5 H5B 108.0 . . ? C3 C5 H5B 108.0 . . ? H5A C5 H5B 107.2 . . ? C7 C6 C5 111.7(2) . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C8 113.3(3) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C9 113.6(3) . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 110.3(3) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C3 116.2(2) . . ? C12 C11 H11A 108.2 . . ? C3 C11 H11A 108.2 . . ? C12 C11 H11B 108.2 . . ? C3 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? C13 C12 C11 112.0(2) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 C13 C12 113.9(2) . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13B 108.8 . . ? C12 C13 H13B 108.8 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C15 113.3(3) . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14B 108.9 . . ? C15 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C14 112.7(3) . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C19 119.2(2) . . ? C18 C17 C1 120.7(2) . . ? C19 C17 C1 120.1(2) . . ? C19 C18 C17 120.7(2) 2_456 . ? C19 C18 H18 119.6 2_456 . ? C17 C18 H18 119.6 . . ? C18 C19 C17 120.0(2) 2_456 . ? C18 C19 H19 120.0 2_456 . ? C17 C19 H19 120.0 . . ? C21 Ag1 C20 178.26(12) . . ? N3 C20 Ag1 177.5(3) . . ? N4 C21 Ag1 177.9(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.702 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.081 # Attachment '1D Au(CN)2 C12 (970).cif' data_e970a _database_code_depnum_ccdc_archive 'CCDC 790493' #TrackingRef '1D Au(CN)2 C12 (970).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H116 N4, 2(C2 Au N2)' _chemical_formula_sum 'C66 H116 Au2 N8' _chemical_formula_weight 1415.60 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.417(3) _cell_length_b 10.601(4) _cell_length_c 38.544(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.129(11) _cell_angle_gamma 90.00 _cell_volume 3426(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1040 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 17.82 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1452 _exptl_absorpt_coefficient_mu 4.320 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8130 _exptl_absorpt_correction_T_max 0.8462 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 13945 _diffrn_reflns_av_R_equivalents 0.0713 _diffrn_reflns_av_sigmaI/netI 0.1663 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.27 _reflns_number_total 7662 _reflns_number_gt 3680 _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7662 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1530 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1001 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.003 _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 C1 C 0.6722(9) 0.1837(7) 0.96377(17) 0.0215(18) Uani 1 1 d . . . N1 N 0.6087(7) 0.2967(6) 0.95678(13) 0.0250(15) Uani 1 1 d . . . H1 H 0.5168 0.3146 0.9649 0.030 Uiso 1 1 calc R . . C2 C 0.6827(9) 0.3926(7) 0.93653(17) 0.029(2) Uani 1 1 d . . . H2A H 0.7422 0.4529 0.9524 0.034 Uiso 1 1 calc R . . H2B H 0.5992 0.4400 0.9222 0.034 Uiso 1 1 calc R . . C3 C 0.7977(8) 0.3306(7) 0.91260(17) 0.026(2) Uani 1 1 d . . . C4 C 0.9061(9) 0.2435(7) 0.93504(18) 0.0267(19) Uani 1 1 d . . . H4A H 0.9769 0.1974 0.9202 0.032 Uiso 1 1 calc R . . H4B H 0.9738 0.2938 0.9522 0.032 Uiso 1 1 calc R . . N2 N 0.8126(7) 0.1542(6) 0.95311(13) 0.0255(14) Uani 1 1 d . . . H2 H 0.8505 0.0777 0.9571 0.031 Uiso 1 1 calc R . . C5 C 0.7031(9) 0.2559(7) 0.88379(17) 0.029(2) Uani 1 1 d . . . H5A H 0.7771 0.1970 0.8735 0.035 Uiso 1 1 calc R . . H5B H 0.6227 0.2043 0.8946 0.035 Uiso 1 1 calc R . . C6 C 0.6177(9) 0.3330(8) 0.85452(18) 0.036(2) Uani 1 1 d . . . H6A H 0.6979 0.3737 0.8409 0.043 Uiso 1 1 calc R . . H6B H 0.5552 0.4006 0.8647 0.043 Uiso 1 1 calc R . . C7 C 0.5046(9) 0.2517(7) 0.82981(18) 0.037(2) Uani 1 1 d . . . H7A H 0.5613 0.1737 0.8241 0.045 Uiso 1 1 calc R . . H7B H 0.4115 0.2268 0.8422 0.045 Uiso 1 1 calc R . . C8 C 0.4443(9) 0.3182(7) 0.79568(17) 0.032(2) Uani 1 1 d . . . H8A H 0.4012 0.4018 0.8015 0.039 Uiso 1 1 calc R . . H8B H 0.5363 0.3329 0.7819 0.039 Uiso 1 1 calc R . . C9 C 0.3179(9) 0.2482(8) 0.77330(18) 0.033(2) Uani 1 1 d . . . H9A H 0.3571 0.1619 0.7692 0.040 Uiso 1 1 calc R . . H9B H 0.2220 0.2404 0.7863 0.040 Uiso 1 1 calc R . . C10 C 0.2701(9) 0.3079(7) 0.73880(17) 0.032(2) Uani 1 1 d . . . H10A H 0.3633 0.3090 0.7248 0.039 Uiso 1 1 calc R . . H10B H 0.2386 0.3965 0.7426 0.039 Uiso 1 1 calc R . . C11 C 0.1324(9) 0.2396(8) 0.71827(18) 0.036(2) Uani 1 1 d . . . H11A H 0.1600 0.1492 0.7165 0.043 Uiso 1 1 calc R . . H11B H 0.0365 0.2457 0.7313 0.043 Uiso 1 1 calc R . . C12 C 0.0923(9) 0.2917(8) 0.68165(18) 0.034(2) Uani 1 1 d . . . H12A H 0.1840 0.2778 0.6677 0.041 Uiso 1 1 calc R . . H12B H 0.0743 0.3838 0.6830 0.041 Uiso 1 1 calc R . . C13 C -0.0559(9) 0.2294(8) 0.66334(19) 0.042(2) Uani 1 1 d . . . H13A H -0.1480 0.2482 0.6768 0.050 Uiso 1 1 calc R . . H13B H -0.0400 0.1368 0.6638 0.050 Uiso 1 1 calc R . . C14 C -0.0987(9) 0.2705(8) 0.62491(17) 0.036(2) Uani 1 1 d . . . H14A H -0.2083 0.2420 0.6174 0.044 Uiso 1 1 calc R . . H14B H -0.0974 0.3638 0.6237 0.044 Uiso 1 1 calc R . . C15 C 0.0142(9) 0.2184(8) 0.60005(17) 0.036(2) Uani 1 1 d . . . H15A H 0.1221 0.2535 0.6061 0.043 Uiso 1 1 calc R . . H15B H 0.0208 0.1257 0.6028 0.043 Uiso 1 1 calc R . . C16 C -0.0382(10) 0.2495(8) 0.56257(18) 0.047(3) Uani 1 1 d . . . H16A H -0.1452 0.2153 0.5564 0.071 Uiso 1 1 calc R . . H16B H 0.0367 0.2121 0.5474 0.071 Uiso 1 1 calc R . . H16C H -0.0401 0.3413 0.5595 0.071 Uiso 1 1 calc R . . C17 C 0.8958(8) 0.4375(7) 0.89865(17) 0.030(2) Uani 1 1 d . . . H17A H 0.8224 0.4942 0.8845 0.036 Uiso 1 1 calc R . . H17B H 0.9437 0.4870 0.9187 0.036 Uiso 1 1 calc R . . C18 C 1.0282(9) 0.3983(7) 0.87670(18) 0.034(2) Uani 1 1 d . . . H18A H 0.9831 0.3421 0.8578 0.041 Uiso 1 1 calc R . . H18B H 1.1086 0.3493 0.8914 0.041 Uiso 1 1 calc R . . C19 C 1.1115(9) 0.5095(7) 0.86051(18) 0.036(2) Uani 1 1 d . . . H19A H 1.2090 0.4784 0.8507 0.043 Uiso 1 1 calc R . . H19B H 1.1447 0.5711 0.8791 0.043 Uiso 1 1 calc R . . C20 C 1.0056(9) 0.5773(7) 0.83145(19) 0.037(2) Uani 1 1 d . . . H20A H 0.9033 0.5995 0.8408 0.044 Uiso 1 1 calc R . . H20B H 1.0587 0.6572 0.8259 0.044 Uiso 1 1 calc R . . C21 C 0.9679(9) 0.5036(8) 0.79719(18) 0.040(2) Uani 1 1 d . . . H21A H 1.0664 0.4975 0.7850 0.048 Uiso 1 1 calc R . . H21B H 0.9354 0.4168 0.8028 0.048 Uiso 1 1 calc R . . C22 C 0.8360(9) 0.5634(8) 0.77244(18) 0.039(2) Uani 1 1 d . . . H22A H 0.7377 0.5696 0.7846 0.047 Uiso 1 1 calc R . . H22B H 0.8686 0.6502 0.7668 0.047 Uiso 1 1 calc R . . C23 C 0.7988(9) 0.4921(8) 0.73913(19) 0.040(2) Uani 1 1 d . . . H23A H 0.8917 0.4955 0.7251 0.048 Uiso 1 1 calc R . . H23B H 0.7782 0.4025 0.7445 0.048 Uiso 1 1 calc R . . C24 C 0.6544(10) 0.5472(8) 0.71830(18) 0.040(2) Uani 1 1 d . . . H24A H 0.6754 0.6370 0.7133 0.048 Uiso 1 1 calc R . . H24B H 0.5621 0.5438 0.7325 0.048 Uiso 1 1 calc R . . C25 C 0.6114(9) 0.4783(8) 0.68401(19) 0.037(2) Uani 1 1 d . . . H25A H 0.7021 0.4855 0.6694 0.045 Uiso 1 1 calc R . . H25B H 0.5967 0.3876 0.6890 0.045 Uiso 1 1 calc R . . C26 C 0.4619(9) 0.5268(8) 0.66324(18) 0.037(2) Uani 1 1 d . . . H26A H 0.4739 0.6186 0.6595 0.044 Uiso 1 1 calc R . . H26B H 0.3700 0.5146 0.6772 0.044 Uiso 1 1 calc R . . C27 C 0.4237(10) 0.4626(8) 0.62753(18) 0.043(2) Uani 1 1 d . . . H27A H 0.5141 0.4761 0.6132 0.052 Uiso 1 1 calc R . . H27B H 0.4125 0.3706 0.6311 0.052 Uiso 1 1 calc R . . C28 C 0.2704(10) 0.5133(8) 0.6078(2) 0.052(3) Uani 1 1 d . . . H28A H 0.1791 0.4935 0.6209 0.078 Uiso 1 1 calc R . . H28B H 0.2555 0.4738 0.5848 0.078 Uiso 1 1 calc R . . H28C H 0.2788 0.6049 0.6052 0.078 Uiso 1 1 calc R . . C29 C 0.5823(9) 0.0891(7) 0.98206(17) 0.0219(18) Uani 1 1 d . . . C30 C 0.4169(9) 0.0880(7) 0.97810(16) 0.0243(19) Uani 1 1 d . . . H30 H 0.3607 0.1480 0.9634 0.029 Uiso 1 1 calc R . . C31 C 0.3339(9) -0.0012(7) 0.99572(18) 0.027(2) Uani 1 1 d . . . H31 H 0.2206 -0.0030 0.9928 0.032 Uiso 1 1 calc R . . Au1 Au 0.11537(4) 0.64717(3) 0.965694(8) 0.03591(11) Uani 1 1 d . . . C32 C 0.0010(10) 0.8139(8) 0.9600(2) 0.038(2) Uani 1 1 d . . . N3 N 0.3077(8) 0.3946(7) 0.9711(2) 0.053(2) Uani 1 1 d . . . C33 C 0.2378(10) 0.4841(8) 0.9701(2) 0.042(2) Uani 1 1 d . . . N4 N -0.0558(8) 0.9089(7) 0.95616(19) 0.045(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.021(5) 0.018(5) 0.023(4) 0.007(4) -0.014(4) -0.001(3) N1 0.035(4) 0.018(4) 0.022(3) 0.006(3) -0.001(3) 0.006(3) C2 0.044(5) 0.020(5) 0.023(4) 0.007(3) 0.006(4) 0.000(4) C3 0.030(5) 0.027(5) 0.021(4) 0.008(4) 0.006(4) 0.009(4) C4 0.036(5) 0.015(4) 0.030(4) 0.009(4) 0.007(4) -0.001(4) N2 0.024(4) 0.021(4) 0.031(3) 0.009(4) 0.000(3) 0.006(3) C5 0.036(5) 0.028(5) 0.024(4) -0.001(4) -0.001(4) -0.002(4) C6 0.037(5) 0.034(6) 0.037(4) -0.003(5) 0.003(4) -0.004(4) C7 0.046(6) 0.028(5) 0.036(5) 0.003(4) -0.003(5) -0.005(4) C8 0.044(6) 0.030(6) 0.023(4) -0.001(4) 0.002(4) -0.002(4) C9 0.031(5) 0.036(6) 0.030(4) -0.006(4) -0.006(4) -0.001(4) C10 0.040(6) 0.030(5) 0.026(4) 0.002(4) -0.001(4) 0.000(4) C11 0.039(6) 0.033(6) 0.035(5) 0.005(4) -0.003(4) 0.001(4) C12 0.028(5) 0.037(6) 0.035(4) 0.002(4) -0.003(4) -0.001(4) C13 0.028(5) 0.052(7) 0.044(5) 0.000(5) 0.000(5) 0.003(5) C14 0.033(5) 0.043(6) 0.031(4) 0.012(4) -0.010(4) -0.006(4) C15 0.047(6) 0.028(5) 0.033(4) 0.002(4) -0.001(5) -0.002(4) C16 0.064(7) 0.045(6) 0.034(5) 0.001(5) 0.006(5) 0.007(5) C17 0.032(5) 0.032(5) 0.026(4) 0.005(4) 0.003(4) 0.000(4) C18 0.036(5) 0.031(5) 0.037(4) 0.002(4) 0.009(4) -0.004(4) C19 0.036(5) 0.036(6) 0.035(5) 0.013(4) -0.003(4) -0.011(4) C20 0.042(6) 0.025(5) 0.045(5) 0.007(4) 0.012(5) -0.001(4) C21 0.041(6) 0.048(6) 0.033(5) -0.006(5) 0.006(5) 0.005(5) C22 0.041(6) 0.043(6) 0.034(5) 0.005(5) 0.006(4) -0.006(5) C23 0.042(6) 0.051(7) 0.029(4) -0.005(5) 0.008(5) 0.003(5) C24 0.050(6) 0.035(6) 0.034(5) -0.012(5) 0.003(5) -0.004(5) C25 0.040(6) 0.031(5) 0.042(5) 0.009(4) 0.004(5) -0.009(4) C26 0.039(6) 0.036(6) 0.037(5) -0.001(4) 0.007(5) -0.005(5) C27 0.056(6) 0.044(6) 0.030(5) 0.004(5) 0.004(5) -0.004(5) C28 0.063(7) 0.047(7) 0.044(5) 0.001(5) -0.009(5) -0.003(5) C29 0.028(5) 0.013(4) 0.023(4) -0.011(4) -0.001(4) 0.001(4) C30 0.030(5) 0.024(5) 0.018(4) -0.008(4) 0.001(4) 0.001(4) C31 0.023(5) 0.025(5) 0.032(4) -0.016(4) 0.002(4) 0.002(4) Au1 0.0370(2) 0.02589(17) 0.04349(18) -0.0055(2) -0.00398(14) 0.0080(2) C32 0.037(6) 0.037(6) 0.037(5) 0.012(5) -0.012(5) 0.001(5) N3 0.037(5) 0.036(5) 0.087(6) -0.005(5) 0.014(4) 0.014(4) C33 0.046(6) 0.030(6) 0.049(5) -0.001(5) 0.009(5) 0.007(5) N4 0.050(5) 0.026(5) 0.061(5) 0.006(4) 0.010(4) 0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.323(8) . ? C1 N1 1.329(8) . ? C1 C29 1.473(9) . ? N1 C2 1.455(8) . ? N1 H1 0.8800 . ? C2 C3 1.542(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.514(9) . ? C3 C5 1.528(9) . ? C3 C17 1.529(9) . ? C4 N2 1.448(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.521(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.547(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.538(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.505(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.495(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.526(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.525(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.528(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.555(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.513(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.509(9) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.516(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.533(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.545(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.543(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.535(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.498(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.513(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.525(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.520(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.543(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.535(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.387(9) . ? C29 C31 1.411(9) 3_657 ? C30 C31 1.389(9) . ? C30 H30 0.9500 . ? C31 C29 1.411(9) 3_657 ? C31 H31 0.9500 . ? Au1 C33 2.012(9) . ? Au1 C32 2.015(9) . ? C32 N4 1.119(9) . ? N3 C33 1.115(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 120.3(7) . . ? N2 C1 C29 119.9(7) . . ? N1 C1 C29 119.8(7) . . ? C1 N1 C2 123.7(6) . . ? C1 N1 H1 118.2 . . ? C2 N1 H1 118.2 . . ? N1 C2 C3 110.2(6) . . ? N1 C2 H2A 109.6 . . ? C3 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C5 110.3(7) . . ? C4 C3 C17 109.6(6) . . ? C5 C3 C17 113.1(5) . . ? C4 C3 C2 107.2(5) . . ? C5 C3 C2 110.0(6) . . ? C17 C3 C2 106.4(6) . . ? N2 C4 C3 110.4(6) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 122.2(7) . . ? C1 N2 H2 118.9 . . ? C4 N2 H2 118.9 . . ? C6 C5 C3 116.2(7) . . ? C6 C5 H5A 108.2 . . ? C3 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? C3 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 112.4(7) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 114.1(7) . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 115.3(7) . . ? C9 C8 H8A 108.5 . . ? C7 C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? C7 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C8 114.9(7) . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? C8 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 C10 C11 113.0(6) . . ? C9 C10 H10A 109.0 . . ? C11 C10 H10A 109.0 . . ? C9 C10 H10B 109.0 . . ? C11 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C10 113.8(6) . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11B 108.8 . . ? C10 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C11 C12 C13 112.0(7) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C14 115.4(7) . . ? C12 C13 H13A 108.4 . . ? C14 C13 H13A 108.4 . . ? C12 C13 H13B 108.4 . . ? C14 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C13 113.3(6) . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C14 112.4(6) . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C14 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C3 116.1(6) . . ? C18 C17 H17A 108.3 . . ? C3 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? C3 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C17 C18 C19 113.7(6) . . ? C17 C18 H18A 108.8 . . ? C19 C18 H18A 108.8 . . ? C17 C18 H18B 108.8 . . ? C19 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C18 C19 C20 113.4(6) . . ? C18 C19 H19A 108.9 . . ? C20 C19 H19A 108.9 . . ? C18 C19 H19B 108.9 . . ? C20 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C21 C20 C19 116.5(7) . . ? C21 C20 H20A 108.2 . . ? C19 C20 H20A 108.2 . . ? C21 C20 H20B 108.2 . . ? C19 C20 H20B 108.2 . . ? H20A C20 H20B 107.3 . . ? C22 C21 C20 113.9(7) . . ? C22 C21 H21A 108.8 . . ? C20 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? C20 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C21 114.1(7) . . ? C23 C22 H22A 108.7 . . ? C21 C22 H22A 108.7 . . ? C23 C22 H22B 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C24 C23 C22 110.9(7) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C25 113.1(7) . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C24 114.6(7) . . ? C26 C25 H25A 108.6 . . ? C24 C25 H25A 108.6 . . ? C26 C25 H25B 108.6 . . ? C24 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C25 C26 C27 114.7(7) . . ? C25 C26 H26A 108.6 . . ? C27 C26 H26A 108.6 . . ? C25 C26 H26B 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C26 112.7(7) . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? 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 . . ? C30 C29 C31 120.2(7) . 3_657 ? C30 C29 C1 120.4(7) . . ? C31 C29 C1 119.3(7) 3_657 . ? C29 C30 C31 119.8(7) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C30 C31 C29 120.0(7) . 3_657 ? C30 C31 H31 120.0 . . ? C29 C31 H31 120.0 3_657 . ? C33 Au1 C32 177.3(4) . . ? N4 C32 Au1 176.4(9) . . ? N3 C33 Au1 176.8(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.27 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.257 _refine_diff_density_min -2.467 _refine_diff_density_rms 0.194 # Attachment '1D Au(CN)2 C6 (420).cif' data_e420a _database_code_depnum_ccdc_archive 'CCDC 790494' #TrackingRef '1D Au(CN)2 C6 (420).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H68 N4, 2(C2 Au N2)' _chemical_formula_sum 'C42 H68 Au2 N8' _chemical_formula_weight 1078.98 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5286(13) _cell_length_b 12.843(3) _cell_length_c 13.746(3) _cell_angle_alpha 89.31(3) _cell_angle_beta 83.39(3) _cell_angle_gamma 81.26(3) _cell_volume 1131.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(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 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 6.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6960 _exptl_absorpt_correction_T_max 0.7366 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 12977 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 29.72 _reflns_number_total 6275 _reflns_number_gt 4954 _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^)+(0.0292P)^2^+0.0600P] 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 6275 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 C1 C 0.3523(5) 0.8999(3) 0.5927(2) 0.0224(7) Uani 1 1 d . . . N1 N 0.4613(4) 0.9581(2) 0.6376(2) 0.0244(6) Uani 1 1 d . . . H1 H 0.4288 1.0271 0.6361 0.029 Uiso 1 1 calc R . . C2 C 0.6363(5) 0.9113(3) 0.6904(3) 0.0244(7) Uani 1 1 d . . . H2A H 0.6446 0.9566 0.7472 0.029 Uiso 1 1 calc R . . H2B H 0.7684 0.9082 0.6465 0.029 Uiso 1 1 calc R . . C3 C 0.6103(5) 0.8010(3) 0.7260(3) 0.0232(7) Uani 1 1 d . . . C4 C 0.5718(5) 0.7403(3) 0.6360(3) 0.0256(8) Uani 1 1 d . . . H4A H 0.6986 0.7315 0.5880 0.031 Uiso 1 1 calc R . . H4B H 0.5413 0.6694 0.6559 0.031 Uiso 1 1 calc R . . N2 N 0.3957(5) 0.7976(2) 0.5906(2) 0.0238(6) Uani 1 1 d . . . H2 H 0.3166 0.7616 0.5609 0.029 Uiso 1 1 calc R . . C5 C 0.1706(5) 0.9520(3) 0.5442(2) 0.0215(7) Uani 1 1 d . . . C6 C 0.0672(5) 1.0500(3) 0.5770(2) 0.0230(7) Uani 1 1 d . . . H6 H 0.1135 1.0843 0.6294 0.028 Uiso 1 1 calc R . . C7 C 0.1043(5) 0.9022(3) 0.4670(2) 0.0237(7) Uani 1 1 d . . . H7 H 0.1761 0.8355 0.4442 0.028 Uiso 1 1 calc R . . C8 C 0.8196(5) 0.7520(3) 0.7611(3) 0.0268(8) Uani 1 1 d . . . H8A H 0.9323 0.7578 0.7075 0.032 Uiso 1 1 calc R . . H8B H 0.8451 0.7943 0.8169 0.032 Uiso 1 1 calc R . . C9 C 0.8358(6) 0.6381(3) 0.7924(3) 0.0311(9) Uani 1 1 d . . . H9A H 0.8143 0.5944 0.7367 0.037 Uiso 1 1 calc R . . H9B H 0.7245 0.6310 0.8463 0.037 Uiso 1 1 calc R . . C10 C 1.0481(6) 0.5979(3) 0.8266(3) 0.0309(9) Uani 1 1 d . . . H10A H 1.1588 0.6078 0.7733 0.037 Uiso 1 1 calc R . . H10B H 1.0671 0.6410 0.8833 0.037 Uiso 1 1 calc R . . C11 C 1.0744(6) 0.4831(3) 0.8559(3) 0.0355(9) Uani 1 1 d . . . H11A H 1.0522 0.4400 0.8000 0.043 Uiso 1 1 calc R . . H11B H 0.9668 0.4733 0.9107 0.043 Uiso 1 1 calc R . . C12 C 1.2907(7) 0.4444(4) 0.8871(4) 0.0527(13) Uani 1 1 d . . . H12A H 1.3983 0.4521 0.8317 0.063 Uiso 1 1 calc R . . H12B H 1.3146 0.4888 0.9419 0.063 Uiso 1 1 calc R . . C13 C 1.3130(9) 0.3308(4) 0.9189(4) 0.0677(17) Uani 1 1 d . . . H13A H 1.2038 0.3224 0.9723 0.102 Uiso 1 1 calc R . . H13B H 1.4503 0.3102 0.9415 0.102 Uiso 1 1 calc R . . H13C H 1.2996 0.2861 0.8634 0.102 Uiso 1 1 calc R . . C14 C 0.4249(5) 0.8015(3) 0.8044(2) 0.0226(7) Uani 1 1 d . . . H14A H 0.2964 0.8280 0.7743 0.027 Uiso 1 1 calc R . . H14B H 0.4169 0.7277 0.8241 0.027 Uiso 1 1 calc R . . C15 C 0.4245(6) 0.8659(3) 0.8964(3) 0.0300(8) Uani 1 1 d . . . H15A H 0.5570 0.8443 0.9248 0.036 Uiso 1 1 calc R . . H15B H 0.4158 0.9413 0.8791 0.036 Uiso 1 1 calc R . . C16 C 0.2432(6) 0.8515(3) 0.9722(3) 0.0325(9) Uani 1 1 d . . . H16A H 0.1113 0.8706 0.9427 0.039 Uiso 1 1 calc R . . H16B H 0.2547 0.7762 0.9907 0.039 Uiso 1 1 calc R . . C17 C 0.2347(7) 0.9174(3) 1.0635(3) 0.0400(10) Uani 1 1 d . . . H17A H 0.2093 0.9928 1.0458 0.048 Uiso 1 1 calc R . . H17B H 0.3719 0.9034 1.0891 0.048 Uiso 1 1 calc R . . C18 C 0.0663(8) 0.8958(4) 1.1441(3) 0.0484(12) Uani 1 1 d . . . H18A H -0.0659 0.8952 1.1154 0.058 Uiso 1 1 calc R . . H18B H 0.0429 0.9537 1.1930 0.058 Uiso 1 1 calc R . . C19 C 0.1226(9) 0.7914(5) 1.1957(4) 0.0614(15) Uani 1 1 d . . . H19A H 0.1489 0.7339 1.1475 0.092 Uiso 1 1 calc R . . H19B H 0.0070 0.7799 1.2447 0.092 Uiso 1 1 calc R . . H19C H 0.2483 0.7932 1.2280 0.092 Uiso 1 1 calc R . . Au1 Au 0.28306(2) 0.414688(12) 0.595401(12) 0.03359(6) Uani 1 1 d . . . C20 C 0.1958(7) 0.5624(3) 0.5597(3) 0.0361(9) Uani 1 1 d . . . N3 N 0.1479(6) 0.6491(3) 0.5410(3) 0.0429(9) Uani 1 1 d . . . C21 C 0.3707(6) 0.2672(3) 0.6320(3) 0.0334(9) Uani 1 1 d . . . N4 N 0.4191(5) 0.1816(3) 0.6508(3) 0.0398(8) 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 C1 0.0211(15) 0.0262(18) 0.0189(16) 0.0024(13) -0.0003(12) -0.0023(14) N1 0.0240(14) 0.0192(15) 0.0318(16) 0.0036(12) -0.0085(12) -0.0054(12) C2 0.0205(16) 0.0273(19) 0.0274(18) 0.0046(14) -0.0069(13) -0.0073(14) C3 0.0215(16) 0.0234(17) 0.0256(17) 0.0012(14) -0.0060(13) -0.0039(14) C4 0.0252(17) 0.0246(18) 0.0266(18) 0.0005(14) -0.0071(14) 0.0005(15) N2 0.0259(15) 0.0220(15) 0.0241(15) -0.0010(12) -0.0093(12) -0.0010(12) C5 0.0184(15) 0.0245(18) 0.0208(16) 0.0048(13) -0.0001(12) -0.0029(13) C6 0.0245(17) 0.0250(18) 0.0199(16) 0.0026(13) -0.0044(13) -0.0044(14) C7 0.0265(17) 0.0217(17) 0.0212(16) 0.0026(13) -0.0003(13) -0.0003(14) C8 0.0222(17) 0.0291(19) 0.0294(19) 0.0013(15) -0.0058(14) -0.0030(15) C9 0.0252(18) 0.032(2) 0.037(2) 0.0030(16) -0.0123(15) -0.0026(16) C10 0.0251(18) 0.033(2) 0.034(2) 0.0011(16) -0.0091(15) 0.0012(16) C11 0.030(2) 0.039(2) 0.035(2) 0.0085(18) -0.0078(16) 0.0027(17) C12 0.043(3) 0.058(3) 0.051(3) 0.007(2) -0.014(2) 0.016(2) C13 0.071(4) 0.068(4) 0.053(3) 0.014(3) -0.012(3) 0.029(3) C14 0.0202(16) 0.0223(17) 0.0264(17) 0.0041(14) -0.0028(13) -0.0072(13) C15 0.0316(19) 0.032(2) 0.0267(18) -0.0015(15) -0.0018(15) -0.0070(16) C16 0.032(2) 0.035(2) 0.030(2) -0.0013(16) -0.0022(15) -0.0056(17) C17 0.042(2) 0.040(2) 0.037(2) -0.0083(18) 0.0020(18) -0.0065(19) C18 0.048(3) 0.056(3) 0.039(2) -0.010(2) 0.011(2) -0.013(2) C19 0.062(3) 0.079(4) 0.037(3) -0.006(3) 0.015(2) -0.007(3) Au1 0.03998(10) 0.02430(8) 0.03565(9) -0.00401(6) -0.00104(6) -0.00433(6) C20 0.040(2) 0.032(2) 0.038(2) -0.0044(18) -0.0087(18) -0.0081(18) N3 0.051(2) 0.031(2) 0.050(2) 0.0006(16) -0.0120(18) -0.0104(17) C21 0.0288(19) 0.029(2) 0.041(2) -0.0060(17) 0.0019(16) -0.0038(16) N4 0.0373(19) 0.0293(19) 0.052(2) -0.0058(16) 0.0001(16) -0.0056(15) _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 C1 N2 1.300(4) . ? C1 N1 1.311(5) . ? C1 C5 1.494(4) . ? N1 C2 1.471(4) . ? N1 H1 0.8800 . ? C2 C3 1.521(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C14 1.524(5) . ? C3 C4 1.535(5) . ? C3 C8 1.543(4) . ? C4 N2 1.466(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.389(5) . ? C5 C7 1.389(5) . ? C6 C7 1.391(5) 2_576 ? C6 H6 0.9500 . ? C7 C6 1.391(4) 2_576 ? C7 H7 0.9500 . ? C8 C9 1.511(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.528(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.513(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.532(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.508(7) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.519(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.515(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.514(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.523(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.525(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Au1 C20 1.969(4) . ? Au1 C21 1.971(4) . ? C20 N3 1.144(5) . ? C21 N4 1.131(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 121.8(3) . . ? N2 C1 C5 118.9(3) . . ? N1 C1 C5 119.2(3) . . ? C1 N1 C2 121.9(3) . . ? C1 N1 H1 119.1 . . ? C2 N1 H1 119.1 . . ? N1 C2 C3 111.4(3) . . ? N1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C14 112.2(3) . . ? C2 C3 C4 106.0(3) . . ? C14 C3 C4 108.9(3) . . ? C2 C3 C8 106.7(3) . . ? C14 C3 C8 113.2(3) . . ? C4 C3 C8 109.5(3) . . ? N2 C4 C3 110.0(3) . . ? N2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? N2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C1 N2 C4 122.4(3) . . ? C1 N2 H2 118.8 . . ? C4 N2 H2 118.8 . . ? C6 C5 C7 120.1(3) . . ? C6 C5 C1 119.8(3) . . ? C7 C5 C1 120.0(3) . . ? C5 C6 C7 119.8(3) . 2_576 ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 2_576 . ? C5 C7 C6 120.0(3) . 2_576 ? C5 C7 H7 120.0 . . ? C6 C7 H7 120.0 2_576 . ? C9 C8 C3 116.0(3) . . ? C9 C8 H8A 108.3 . . ? C3 C8 H8A 108.3 . . ? C9 C8 H8B 108.3 . . ? C3 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? C8 C9 C10 111.6(3) . . ? C8 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 113.6(3) . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C10 C11 C12 112.4(4) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C11 111.9(5) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C3 117.1(3) . . ? C15 C14 H14A 108.0 . . ? C3 C14 H14A 108.0 . . ? C15 C14 H14B 108.0 . . ? C3 C14 H14B 108.0 . . ? H14A C14 H14B 107.3 . . ? C16 C15 C14 111.8(3) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 113.0(3) . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C15 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? C16 C17 C18 113.5(4) . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17B 108.9 . . ? C18 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C17 C18 C19 112.7(4) . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? C19 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 Au1 C21 179.63(16) . . ? N3 C20 Au1 178.1(4) . . ? N4 C21 Au1 178.2(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.72 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.981 _refine_diff_density_min -1.224 _refine_diff_density_rms 0.137 # Attachment '2D Ag(CN)2 C12 (988).cif' data_e988a _database_code_depnum_ccdc_archive 'CCDC 790495' #TrackingRef '2D Ag(CN)2 C12 (988).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H116 N4, 2(C2 Ag N2)' _chemical_formula_sum 'C66 H116 Ag2 N8' _chemical_formula_weight 1237.41 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.6481(3) _cell_length_b 11.9345(6) _cell_length_c 22.3115(10) _cell_angle_alpha 78.366(3) _cell_angle_beta 88.925(4) _cell_angle_gamma 85.506(3) _cell_volume 1728.53(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1323 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9143 _exptl_absorpt_correction_T_max 0.9417 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 12355 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.1061 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7315 _reflns_number_gt 3835 _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^)+(0.0261P)^2^+0.7445P] 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 7315 _refine_ls_number_parameters 326 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1269 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1155 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.003 _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 C1 C 0.6503(6) 0.5264(4) 0.07450(18) 0.0217(10) Uani 1 1 d . . . N1 N 0.5217(5) 0.4459(3) 0.08495(15) 0.0227(8) Uani 1 1 d . . . H1 H 0.5409 0.3881 0.0659 0.027 Uiso 1 1 calc R . . C2 C 0.3491(6) 0.4474(4) 0.12628(19) 0.0245(10) Uani 1 1 d . . . H2A H 0.3275 0.3679 0.1473 0.029 Uiso 1 1 calc R . . H2B H 0.2265 0.4789 0.1023 0.029 Uiso 1 1 calc R . . C3 C 0.3816(6) 0.5202(3) 0.17415(18) 0.0207(9) Uani 1 1 d . . . C4 C 0.4457(6) 0.6361(3) 0.13774(19) 0.0238(10) Uani 1 1 d . . . H4A H 0.3326 0.6761 0.1117 0.029 Uiso 1 1 calc R . . H4B H 0.4792 0.6852 0.1664 0.029 Uiso 1 1 calc R . . N2 N 0.6205(5) 0.6175(3) 0.09961(15) 0.0233(8) Uani 1 1 d . . . H2 H 0.7101 0.6692 0.0930 0.028 Uiso 1 1 calc R . . C5 C 0.5526(6) 0.4664(4) 0.21867(19) 0.0240(10) Uani 1 1 d . . . H5A H 0.6793 0.4658 0.1947 0.029 Uiso 1 1 calc R . . H5B H 0.5671 0.5182 0.2476 0.029 Uiso 1 1 calc R . . C6 C 0.5363(7) 0.3462(4) 0.2562(2) 0.0340(12) Uani 1 1 d . . . H6A H 0.5252 0.2918 0.2285 0.041 Uiso 1 1 calc R . . H6B H 0.4132 0.3446 0.2820 0.041 Uiso 1 1 calc R . . C7 C 0.7225(7) 0.3093(4) 0.2971(2) 0.0367(12) Uani 1 1 d . . . H7A H 0.8444 0.3267 0.2718 0.044 Uiso 1 1 calc R . . H7B H 0.7184 0.3565 0.3289 0.044 Uiso 1 1 calc R . . C8 C 0.7438(7) 0.1835(4) 0.3285(2) 0.0390(13) Uani 1 1 d . . . H8A H 0.6282 0.1666 0.3566 0.047 Uiso 1 1 calc R . . H8B H 0.7400 0.1354 0.2973 0.047 Uiso 1 1 calc R . . C9 C 0.9391(7) 0.1525(4) 0.3645(2) 0.0358(12) Uani 1 1 d . . . H9A H 1.0532 0.1761 0.3369 0.043 Uiso 1 1 calc R . . H9B H 0.9372 0.1970 0.3975 0.043 Uiso 1 1 calc R . . C10 C 0.9769(7) 0.0262(4) 0.3928(2) 0.0366(12) Uani 1 1 d . . . H10A H 0.9774 -0.0186 0.3600 0.044 Uiso 1 1 calc R . . H10B H 0.8642 0.0026 0.4210 0.044 Uiso 1 1 calc R . . C11 C 1.1747(7) -0.0036(4) 0.4280(2) 0.0366(12) Uani 1 1 d . . . H11A H 1.2871 0.0219 0.4001 0.044 Uiso 1 1 calc R . . H11B H 1.1727 0.0396 0.4615 0.044 Uiso 1 1 calc R . . C12 C 1.2156(7) -0.1306(4) 0.4550(2) 0.0358(12) Uani 1 1 d . . . H12A H 1.1035 -0.1563 0.4830 0.043 Uiso 1 1 calc R . . H12B H 1.2183 -0.1740 0.4216 0.043 Uiso 1 1 calc R . . C13 C 1.4133(7) -0.1585(4) 0.4900(2) 0.0368(12) Uani 1 1 d . . . H13A H 1.4085 -0.1166 0.5241 0.044 Uiso 1 1 calc R . . H13B H 1.5245 -0.1302 0.4623 0.044 Uiso 1 1 calc R . . C14 C 1.4607(7) -0.2856(4) 0.5159(2) 0.0410(13) Uani 1 1 d . . . H14A H 1.3512 -0.3138 0.5443 0.049 Uiso 1 1 calc R . . H14B H 1.4635 -0.3279 0.4820 0.049 Uiso 1 1 calc R . . C15 C 1.6603(8) -0.3117(5) 0.5496(3) 0.0550(16) Uani 1 1 d . . . H15A H 1.6549 -0.2718 0.5845 0.066 Uiso 1 1 calc R . . H15B H 1.7686 -0.2802 0.5216 0.066 Uiso 1 1 calc R . . C16 C 1.7147(10) -0.4386(5) 0.5734(3) 0.0550(16) Uani 1 1 d . . . H16A H 1.6138 -0.4695 0.6036 0.066 Uiso 1 1 calc R . . H16B H 1.8479 -0.4490 0.5927 0.066 Uiso 1 1 calc R . . H16C H 1.7173 -0.4793 0.5394 0.066 Uiso 1 1 calc R . . C17 C 0.1780(6) 0.5371(4) 0.20581(19) 0.0251(10) Uani 1 1 d . . . H17A H 0.0767 0.5712 0.1741 0.030 Uiso 1 1 calc R . . H17B H 0.1356 0.4607 0.2258 0.030 Uiso 1 1 calc R . . C18 C 0.1747(6) 0.6123(4) 0.2536(2) 0.0315(11) Uani 1 1 d . . . H18A H 0.2745 0.5784 0.2858 0.038 Uiso 1 1 calc R . . H18B H 0.2155 0.6892 0.2339 0.038 Uiso 1 1 calc R . . C19 C -0.0314(6) 0.6251(4) 0.2829(2) 0.0325(11) Uani 1 1 d . . . H19A H -0.0738 0.5479 0.3014 0.039 Uiso 1 1 calc R . . H19B H -0.1303 0.6609 0.2507 0.039 Uiso 1 1 calc R . . C20 C -0.0351(7) 0.6973(4) 0.3320(2) 0.0389(12) Uani 1 1 d . . . H20A H -0.0048 0.7764 0.3126 0.047 Uiso 1 1 calc R . . H20B H 0.0727 0.6656 0.3620 0.047 Uiso 1 1 calc R . . C21 C -0.2365(8) 0.7020(5) 0.3659(2) 0.0513(15) Uani 1 1 d . . . H21A H -0.2660 0.6227 0.3850 0.062 Uiso 1 1 calc R . . H21B H -0.2220 0.7443 0.3993 0.062 Uiso 1 1 calc R . . C22 C -0.4147(10) 0.7577(6) 0.3272(3) 0.0835(10) Uani 1 1 d . . . H22A H -0.4241 0.7196 0.2919 0.100 Uiso 1 1 calc R . . H22B H -0.5396 0.7453 0.3517 0.100 Uiso 1 1 calc R . . C23 C -0.4030(9) 0.8841(6) 0.3037(3) 0.0835(10) Uani 1 1 d D B . H23A H -0.2877 0.8950 0.2750 0.100 Uiso 1 1 calc R . . H23B H -0.3735 0.9197 0.3387 0.100 Uiso 1 1 calc R . . C24 C -0.5878(9) 0.9475(6) 0.2718(3) 0.0835(10) Uani 1 1 d D . . H24A H -0.7087 0.9163 0.2936 0.100 Uiso 1 1 calc R A 1 H24B H -0.5891 1.0292 0.2749 0.100 Uiso 1 1 calc R A 1 C25 C -0.6030(12) 0.9413(9) 0.2073(3) 0.0835(10) Uani 0.731(6) 1 d PD B 1 H25A H -0.6399 0.8636 0.2050 0.100 Uiso 0.731(6) 1 calc PR B 1 H25B H -0.4680 0.9509 0.1884 0.100 Uiso 0.731(6) 1 calc PR B 1 C26 C -0.7549(13) 1.0294(9) 0.1691(4) 0.0835(10) Uani 0.731(6) 1 d PD B 1 H26A H -0.6956 1.1045 0.1611 0.100 Uiso 0.731(6) 1 calc PR B 1 H26B H -0.7691 1.0070 0.1291 0.100 Uiso 0.731(6) 1 calc PR B 1 C27 C -0.9538(12) 1.0455(9) 0.1937(4) 0.0835(10) Uani 0.731(6) 1 d PD B 1 H27A H -0.9436 1.0665 0.2342 0.100 Uiso 0.731(6) 1 calc PR B 1 H27B H -1.0199 0.9725 0.1996 0.100 Uiso 0.731(6) 1 calc PR B 1 C28 C -1.0831(13) 1.1396(10) 0.1513(5) 0.0835(10) Uani 0.731(6) 1 d PD B 1 H28A H -1.0735 1.2131 0.1639 0.125 Uiso 0.731(6) 1 calc PR B 1 H28B H -1.2241 1.1203 0.1537 0.125 Uiso 0.731(6) 1 calc PR B 1 H28C H -1.0346 1.1456 0.1091 0.125 Uiso 0.731(6) 1 calc PR B 1 C25A C -0.588(2) 1.0366(19) 0.2146(8) 0.0835(10) Uani 0.269(6) 1 d PD B 2 H25C H -0.4862 1.0107 0.1864 0.100 Uiso 0.269(6) 1 calc PR B 2 H25D H -0.5442 1.1079 0.2248 0.100 Uiso 0.269(6) 1 calc PR B 2 C26A C -0.790(3) 1.066(2) 0.1804(10) 0.0835(10) Uani 0.269(6) 1 d PD B 2 H26C H -0.7568 1.0718 0.1364 0.100 Uiso 0.269(6) 1 calc PR B 2 H26D H -0.8673 0.9971 0.1924 0.100 Uiso 0.269(6) 1 calc PR B 2 C27A C -0.924(3) 1.159(2) 0.1838(12) 0.0835(10) Uani 0.269(6) 1 d PD B 2 H27C H -0.8764 1.2276 0.1558 0.100 Uiso 0.269(6) 1 calc PR B 2 H27D H -0.9198 1.1741 0.2259 0.100 Uiso 0.269(6) 1 calc PR B 2 C28A C -1.151(3) 1.149(3) 0.1678(14) 0.0835(10) Uani 0.269(6) 1 d PD B 2 H28D H -1.1554 1.0999 0.1374 0.125 Uiso 0.269(6) 1 calc PR B 2 H28E H -1.2151 1.2248 0.1511 0.125 Uiso 0.269(6) 1 calc PR B 2 H28F H -1.2221 1.1141 0.2049 0.125 Uiso 0.269(6) 1 calc PR B 2 C29 C 0.8300(6) 0.5131(4) 0.03591(18) 0.0202(9) Uani 1 1 d . . . C30 C 0.9116(6) 0.4041(4) 0.03139(18) 0.0243(10) Uani 1 1 d . . . H30 H 0.8498 0.3384 0.0527 0.029 Uiso 1 1 calc R . . C31 C 1.0805(6) 0.3906(4) -0.00358(19) 0.0243(10) Uani 1 1 d . . . H31 H 1.1364 0.3158 -0.0058 0.029 Uiso 1 1 calc R . . Ag1 Ag 0.5000 0.0000 0.0000 0.04013(19) Uani 1 2 d S . . Ag2 Ag 0.0000 0.0000 0.0000 0.04184(19) Uani 1 2 d S . . N3 N 0.5262(6) 0.2417(3) 0.03891(19) 0.0408(11) Uani 1 1 d . . . N4 N -0.0993(7) -0.2123(4) 0.1060(2) 0.0486(12) Uani 1 1 d . . . C32 C 0.5190(7) 0.1569(4) 0.0251(2) 0.0335(12) Uani 1 1 d . . . C33 C -0.0594(7) -0.1351(5) 0.0701(3) 0.0414(13) 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 C1 0.024(2) 0.020(2) 0.022(2) -0.0068(19) -0.0018(19) -0.003(2) N1 0.024(2) 0.0173(19) 0.030(2) -0.0132(16) 0.0040(16) -0.0014(16) C2 0.022(2) 0.023(2) 0.032(2) -0.011(2) 0.0040(19) -0.005(2) C3 0.020(2) 0.016(2) 0.027(2) -0.0077(19) 0.0011(19) -0.0013(19) C4 0.021(2) 0.019(2) 0.032(3) -0.010(2) 0.0051(19) -0.002(2) N2 0.024(2) 0.0191(19) 0.028(2) -0.0074(16) 0.0085(16) -0.0072(17) C5 0.023(2) 0.023(2) 0.026(2) -0.006(2) -0.0014(19) -0.002(2) C6 0.034(3) 0.031(3) 0.036(3) -0.003(2) -0.005(2) -0.005(2) C7 0.037(3) 0.031(3) 0.039(3) 0.001(2) -0.009(2) -0.004(2) C8 0.043(3) 0.031(3) 0.040(3) 0.000(2) -0.006(2) 0.000(2) C9 0.038(3) 0.029(3) 0.039(3) -0.002(2) -0.009(2) 0.000(2) C10 0.035(3) 0.034(3) 0.040(3) -0.006(2) -0.001(2) 0.002(2) C11 0.039(3) 0.032(3) 0.039(3) -0.006(2) -0.003(2) 0.000(2) C12 0.037(3) 0.032(3) 0.037(3) -0.006(2) -0.004(2) 0.003(2) C13 0.039(3) 0.032(3) 0.039(3) -0.010(2) -0.008(2) 0.005(2) C14 0.049(3) 0.034(3) 0.039(3) -0.009(2) -0.005(2) 0.005(3) C15 0.058(4) 0.040(3) 0.066(4) -0.011(3) -0.018(3) 0.010(3) C16 0.058(4) 0.040(3) 0.066(4) -0.011(3) -0.018(3) 0.010(3) C17 0.021(2) 0.026(2) 0.029(2) -0.009(2) 0.0008(19) -0.003(2) C18 0.029(3) 0.036(3) 0.035(3) -0.017(2) 0.009(2) -0.007(2) C19 0.025(3) 0.036(3) 0.040(3) -0.018(2) 0.008(2) -0.003(2) C20 0.037(3) 0.044(3) 0.039(3) -0.016(3) 0.007(2) -0.004(3) C21 0.064(4) 0.045(3) 0.050(3) -0.019(3) 0.021(3) -0.008(3) C22 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C23 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C24 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C25 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C26 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C27 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C28 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C25A 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C26A 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C27A 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C28A 0.060(2) 0.095(3) 0.093(2) -0.017(2) 0.0034(17) -0.001(2) C29 0.020(2) 0.020(2) 0.023(2) -0.0079(19) 0.0004(18) -0.0041(19) C30 0.027(2) 0.021(2) 0.027(2) -0.0062(19) -0.001(2) -0.007(2) C31 0.028(3) 0.016(2) 0.031(2) -0.0101(19) 0.001(2) -0.001(2) Ag1 0.0427(4) 0.0242(3) 0.0595(4) -0.0220(3) -0.0042(3) -0.0031(3) Ag2 0.0453(4) 0.0305(4) 0.0501(4) -0.0060(3) -0.0035(3) -0.0097(3) N3 0.041(3) 0.025(2) 0.063(3) -0.024(2) -0.003(2) 0.000(2) N4 0.055(3) 0.034(3) 0.059(3) -0.008(2) -0.006(2) -0.018(2) C32 0.026(3) 0.029(3) 0.048(3) -0.015(2) -0.007(2) 0.001(2) C33 0.034(3) 0.033(3) 0.061(4) -0.018(3) -0.005(3) -0.006(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 C1 N1 1.319(5) . ? C1 N2 1.320(5) . ? C1 C29 1.477(6) . ? N1 C2 1.460(5) . ? N1 H1 0.8800 . ? C2 C3 1.534(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C17 1.533(6) . ? C3 C5 1.537(5) . ? C3 C4 1.543(5) . ? C4 N2 1.457(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.520(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.533(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.521(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.520(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.516(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.524(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.519(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.521(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.517(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.518(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.524(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.517(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.523(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.528(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.508(8) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.502(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.503(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.462(7) . ? C24 C25A 1.488(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.535(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.436(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.532(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C25A C26A 1.536(16) . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C26A C27A 1.390(17) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C27A C28A 1.575(18) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29 C30 1.391(5) . ? C29 C31 1.397(5) 2_765 ? C30 C31 1.373(6) . ? C30 H30 0.9500 . ? C31 C29 1.397(5) 2_765 ? C31 H31 0.9500 . ? Ag1 C32 2.073(5) 2_655 ? Ag1 C32 2.073(5) . ? Ag1 Ag2 3.32405(15) . ? Ag1 Ag2 3.32405(15) 1_655 ? Ag2 C33 2.065(6) . ? Ag2 C33 2.065(6) 2 ? Ag2 Ag1 3.32405(15) 1_455 ? N3 C32 1.120(5) . ? N4 C33 1.136(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 N1 C1 N2 119.9(4) . . ? N1 C1 C29 119.9(4) . . ? N2 C1 C29 120.1(4) . . ? C1 N1 C2 123.7(3) . . ? C1 N1 H1 118.2 . . ? C2 N1 H1 118.2 . . ? N1 C2 C3 111.5(3) . . ? N1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C17 C3 C2 107.1(3) . . ? C17 C3 C5 113.6(3) . . ? C2 C3 C5 111.9(3) . . ? C17 C3 C4 110.3(3) . . ? C2 C3 C4 105.7(3) . . ? C5 C3 C4 108.0(3) . . ? N2 C4 C3 110.1(3) . . ? N2 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N2 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.2 . . ? C1 N2 C4 122.8(3) . . ? C1 N2 H2 118.6 . . ? C4 N2 H2 118.6 . . ? C6 C5 C3 118.8(4) . . ? C6 C5 H5A 107.6 . . ? C3 C5 H5A 107.6 . . ? C6 C5 H5B 107.6 . . ? C3 C5 H5B 107.6 . . ? H5A C5 H5B 107.0 . . ? C5 C6 C7 110.2(4) . . ? C5 C6 H6A 109.6 . . ? C7 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? C7 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 115.5(4) . . ? C8 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? C8 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C9 C8 C7 112.1(4) . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C8 114.6(4) . . ? C10 C9 H9A 108.6 . . ? C8 C9 H9A 108.6 . . ? C10 C9 H9B 108.6 . . ? C8 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? C9 C10 C11 113.9(4) . . ? C9 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 114.0(4) . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? C10 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C11 113.2(4) . . ? C13 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 114.2(4) . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C13 113.3(4) . . ? C15 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? C15 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? C14 C15 C16 114.1(5) . . ? C14 C15 H15A 108.7 . . ? C16 C15 H15A 108.7 . . ? C14 C15 H15B 108.7 . . ? C16 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C3 115.7(3) . . ? C18 C17 H17A 108.4 . . ? C3 C17 H17A 108.4 . . ? C18 C17 H17B 108.4 . . ? C3 C17 H17B 108.4 . . ? H17A C17 H17B 107.4 . . ? C19 C18 C17 112.7(4) . . ? C19 C18 H18A 109.1 . . ? C17 C18 H18A 109.1 . . ? C19 C18 H18B 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 113.1(4) . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C19 C20 C21 113.7(4) . . ? C19 C20 H20A 108.8 . . ? C21 C20 H20A 108.8 . . ? C19 C20 H20B 108.8 . . ? C21 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C22 C21 C20 115.5(5) . . ? C22 C21 H21A 108.4 . . ? C20 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? C20 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C21 113.5(6) . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C22 C23 C24 116.1(6) . . ? C22 C23 H23A 108.3 . . ? C24 C23 H23A 108.3 . . ? C22 C23 H23B 108.3 . . ? C24 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C25 C24 C25A 47.7(11) . . ? C25 C24 C23 114.7(6) . . ? C25A C24 C23 125.4(8) . . ? C25 C24 H24A 108.6 . . ? C25A C24 H24A 125.9 . . ? C23 C24 H24A 108.6 . . ? C25 C24 H24B 108.6 . . ? C25A C24 H24B 61.1 . . ? C23 C24 H24B 108.6 . . ? H24A C24 H24B 107.6 . . ? C24 C25 C26 116.0(7) . . ? C24 C25 H25A 108.3 . . ? C26 C25 H25A 108.3 . . ? C24 C25 H25B 108.3 . . ? C26 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? C27 C26 C25 118.1(8) . . ? C27 C26 H26A 107.8 . . ? C25 C26 H26A 107.8 . . ? C27 C26 H26B 107.8 . . ? C25 C26 H26B 107.8 . . ? H26A C26 H26B 107.1 . . ? C26 C27 C28 111.5(8) . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C24 C25A C26A 116.4(14) . . ? C24 C25A H25C 108.2 . . ? C26A C25A H25C 108.2 . . ? C24 C25A H25D 108.2 . . ? C26A C25A H25D 108.2 . . ? H25C C25A H25D 107.3 . . ? C27A C26A C25A 125.2(19) . . ? C27A C26A H26C 106.0 . . ? C25A C26A H26C 106.0 . . ? C27A C26A H26D 106.0 . . ? C25A C26A H26D 106.0 . . ? H26C C26A H26D 106.3 . . ? C26A C27A C28A 116.3(18) . . ? C26A C27A H27C 108.2 . . ? C28A C27A H27C 108.2 . . ? C26A C27A H27D 108.2 . . ? C28A C27A H27D 108.2 . . ? H27C C27A H27D 107.4 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C30 C29 C31 119.4(4) . 2_765 ? C30 C29 C1 120.1(4) . . ? C31 C29 C1 120.5(4) 2_765 . ? C31 C30 C29 120.6(4) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C29 120.0(4) . 2_765 ? C30 C31 H31 120.0 . . ? C29 C31 H31 120.0 2_765 . ? C32 Ag1 C32 180.0 2_655 . ? C32 Ag1 Ag2 82.14(13) 2_655 . ? C32 Ag1 Ag2 97.86(13) . . ? C32 Ag1 Ag2 97.86(13) 2_655 1_655 ? C32 Ag1 Ag2 82.14(13) . 1_655 ? Ag2 Ag1 Ag2 180.0 . 1_655 ? C33 Ag2 C33 180.0 . 2 ? C33 Ag2 Ag1 76.22(13) . 1_455 ? C33 Ag2 Ag1 103.78(13) 2 1_455 ? C33 Ag2 Ag1 103.78(13) . . ? C33 Ag2 Ag1 76.22(13) 2 . ? Ag1 Ag2 Ag1 180.0 1_455 . ? N3 C32 Ag1 179.0(5) . . ? N4 C33 Ag2 175.4(5) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.089 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.094 # Attachment '2D Ag(CN)2 C3 (463).cif' data_e463a _database_code_depnum_ccdc_archive 'CCDC 790496' #TrackingRef '2D Ag(CN)2 C3 (463).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H44 N4, 2(C2 Ag N2)' _chemical_formula_sum 'C30 H44 Ag2 N8' _chemical_formula_weight 732.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5879(2) _cell_length_b 11.3381(4) _cell_length_c 12.2853(4) _cell_angle_alpha 112.8290(10) _cell_angle_beta 91.8580(10) _cell_angle_gamma 104.2740(10) _cell_volume 811.18(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5659 _cell_measurement_theta_min 3.22 _cell_measurement_theta_max 27.41 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 374 _exptl_absorpt_coefficient_mu 1.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9074 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 11943 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3686 _reflns_number_gt 3033 _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^)+(0.0261P)^2^+0.3099P] 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 3686 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.0000 0.5000 1.0000 0.03265(7) Uani 1 2 d S . . Ag2 Ag 0.5000 0.5000 1.0000 0.03401(7) Uani 1 2 d S . . C1 C 0.4502(3) 0.3495(2) 1.05974(17) 0.0331(4) Uani 1 1 d . . . N1 N 0.4370(3) 0.27281(18) 1.10038(15) 0.0364(4) Uani 1 1 d . . . C2 C 0.9934(3) 0.4400(2) 0.81774(17) 0.0336(4) Uani 1 1 d . . . N2 N 0.9897(3) 0.4093(2) 0.71716(14) 0.0399(4) Uani 1 1 d . . . C3 C 0.2270(3) 0.66505(16) 0.60540(14) 0.0183(3) Uani 1 1 d . . . N3 N 0.2478(2) 0.72708(14) 0.72272(12) 0.0208(3) Uani 1 1 d . . . H3 H 0.3423 0.7152 0.7668 0.025 Uiso 1 1 calc R . . C4 C 0.1174(3) 0.81579(17) 0.78226(14) 0.0219(3) Uani 1 1 d . . . H4A H 0.1965 0.8844 0.8600 0.026 Uiso 1 1 calc R . . H4B H -0.0138 0.7632 0.7975 0.026 Uiso 1 1 calc R . . C5 C 0.0604(3) 0.88397(16) 0.70391(14) 0.0188(3) Uani 1 1 d . . . C6 C -0.0425(3) 0.77158(16) 0.58199(14) 0.0205(3) Uani 1 1 d . . . H6A H -0.1827 0.7207 0.5896 0.025 Uiso 1 1 calc R . . H6B H -0.0644 0.8107 0.5247 0.025 Uiso 1 1 calc R . . N4 N 0.0892(2) 0.68083(14) 0.53588(12) 0.0205(3) Uani 1 1 d . . . H4 H 0.0755 0.6349 0.4583 0.025 Uiso 1 1 calc R . . C7 C -0.1086(3) 0.95509(17) 0.75552(15) 0.0231(4) Uani 1 1 d . . . H7A H -0.1692 0.9781 0.6941 0.028 Uiso 1 1 calc R . . H7B H -0.2243 0.8914 0.7708 0.028 Uiso 1 1 calc R . . C8 C -0.0317(3) 1.08189(19) 0.87053(16) 0.0313(4) Uani 1 1 d . . . H8A H 0.0293 1.0606 0.9330 0.038 Uiso 1 1 calc R . . H8B H 0.0811 1.1478 0.8561 0.038 Uiso 1 1 calc R . . C9 C -0.2116(3) 1.1423(2) 0.91418(17) 0.0354(5) Uani 1 1 d . . . H9A H -0.2710 1.1644 0.8528 0.053 Uiso 1 1 calc R . . H9B H -0.1574 1.2234 0.9876 0.053 Uiso 1 1 calc R . . H9C H -0.3220 1.0779 0.9302 0.053 Uiso 1 1 calc R . . C10 C 0.2639(3) 0.98001(17) 0.69509(16) 0.0238(4) Uani 1 1 d . . . H10A H 0.3280 1.0462 0.7768 0.029 Uiso 1 1 calc R . . H10B H 0.3654 0.9282 0.6626 0.029 Uiso 1 1 calc R . . C11 C 0.2372(3) 1.0551(2) 0.6187(2) 0.0404(5) Uani 1 1 d . . . H11A H 0.1296 1.1033 0.6470 0.048 Uiso 1 1 calc R . . H11B H 0.1859 0.9907 0.5349 0.048 Uiso 1 1 calc R . . C12 C 0.4464(4) 1.1549(3) 0.6244(3) 0.0716(10) Uani 1 1 d . . . H12A H 0.4843 1.2278 0.7042 0.107 Uiso 1 1 calc R . . H12B H 0.4305 1.1911 0.5650 0.107 Uiso 1 1 calc R . . H12C H 0.5581 1.1097 0.6077 0.107 Uiso 1 1 calc R . . C13 C 0.3648(3) 0.57812(16) 0.55072(14) 0.0184(3) Uani 1 1 d . . . C14 C 0.4096(3) 0.55551(16) 0.43486(14) 0.0200(3) Uani 1 1 d . . . H14 H 0.3472 0.5929 0.3902 0.024 Uiso 1 1 calc R . . C15 C 0.5448(3) 0.47873(16) 0.38474(14) 0.0208(3) Uani 1 1 d . . . H15 H 0.5758 0.4649 0.3065 0.025 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 0.03565(12) 0.04256(13) 0.01571(9) 0.00999(8) 0.00248(8) 0.00739(9) Ag2 0.03661(12) 0.03747(12) 0.03080(11) 0.01543(9) 0.00172(9) 0.01331(10) C1 0.0322(10) 0.0394(11) 0.0251(9) 0.0087(8) -0.0012(8) 0.0138(9) N1 0.0396(10) 0.0406(10) 0.0292(8) 0.0133(8) -0.0018(7) 0.0139(8) C2 0.0278(10) 0.0457(12) 0.0239(9) 0.0126(8) 0.0006(7) 0.0075(9) N2 0.0342(9) 0.0610(12) 0.0211(8) 0.0142(8) 0.0027(7) 0.0120(9) C3 0.0186(8) 0.0168(7) 0.0188(7) 0.0074(6) 0.0032(6) 0.0032(6) N3 0.0264(7) 0.0229(7) 0.0169(6) 0.0090(6) 0.0026(5) 0.0121(6) C4 0.0272(9) 0.0237(8) 0.0178(7) 0.0086(6) 0.0067(6) 0.0116(7) C5 0.0192(8) 0.0190(8) 0.0179(7) 0.0069(6) 0.0010(6) 0.0060(6) C6 0.0202(8) 0.0220(8) 0.0185(7) 0.0064(6) 0.0005(6) 0.0077(7) N4 0.0225(7) 0.0226(7) 0.0145(6) 0.0039(5) 0.0015(5) 0.0094(6) C7 0.0236(8) 0.0232(8) 0.0219(8) 0.0071(7) 0.0021(7) 0.0095(7) C8 0.0357(10) 0.0290(10) 0.0246(9) 0.0030(8) -0.0013(8) 0.0148(8) C9 0.0465(12) 0.0373(11) 0.0244(9) 0.0070(8) 0.0041(8) 0.0245(10) C10 0.0191(8) 0.0244(8) 0.0284(9) 0.0133(7) -0.0017(7) 0.0036(7) C11 0.0307(10) 0.0450(12) 0.0559(13) 0.0378(11) -0.0029(9) 0.0013(9) C12 0.0479(15) 0.076(2) 0.109(3) 0.078(2) -0.0130(15) -0.0144(14) C13 0.0176(7) 0.0167(7) 0.0195(7) 0.0069(6) 0.0032(6) 0.0036(6) C14 0.0226(8) 0.0204(8) 0.0190(7) 0.0097(6) 0.0026(6) 0.0068(7) C15 0.0235(8) 0.0211(8) 0.0179(7) 0.0084(6) 0.0041(6) 0.0056(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C2 2.0678(19) . ? Ag1 C2 2.0678(19) 2_767 ? Ag2 C1 2.066(2) 2_667 ? Ag2 C1 2.066(2) . ? C1 N1 1.147(3) . ? C2 N2 1.144(2) . ? C3 N4 1.317(2) . ? C3 N3 1.320(2) . ? C3 C13 1.488(2) . ? N3 C4 1.477(2) . ? N3 H3 0.8800 . ? C4 C5 1.537(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.534(2) . ? C5 C10 1.541(2) . ? C5 C7 1.544(2) . ? C6 N4 1.467(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N4 H4 0.8800 . ? C7 C8 1.529(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.522(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.524(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.532(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.398(2) 2_666 ? C13 C14 1.400(2) . ? C14 C15 1.390(2) . ? C14 H14 0.9500 . ? C15 C13 1.398(2) 2_666 ? C15 H15 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 C2 Ag1 C2 180.000(1) . 2_767 ? C2 Ag1 Ag2 84.55(5) . 1_655 ? C2 Ag1 Ag2 95.45(5) 2_767 1_655 ? C2 Ag1 Ag2 95.45(5) . . ? C2 Ag1 Ag2 84.55(5) 2_767 . ? Ag2 Ag1 Ag2 180.0 1_655 . ? C1 Ag2 C1 180.000(1) 2_667 . ? C1 Ag2 Ag1 91.92(5) 2_667 . ? C1 Ag2 Ag1 88.08(5) . . ? C1 Ag2 Ag1 88.08(5) 2_667 1_455 ? C1 Ag2 Ag1 91.92(5) . 1_455 ? Ag1 Ag2 Ag1 180.0 . 1_455 ? N1 C1 Ag2 174.14(17) . . ? N2 C2 Ag1 178.7(2) . . ? N4 C3 N3 121.15(14) . . ? N4 C3 C13 119.40(14) . . ? N3 C3 C13 119.44(14) . . ? C3 N3 C4 122.00(14) . . ? C3 N3 H3 119.0 . . ? C4 N3 H3 119.0 . . ? N3 C4 C5 110.41(13) . . ? N3 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? N3 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 106.16(13) . . ? C4 C5 C10 108.90(13) . . ? C6 C5 C10 112.08(14) . . ? C4 C5 C7 109.76(14) . . ? C6 C5 C7 107.08(13) . . ? C10 C5 C7 112.65(14) . . ? N4 C6 C5 111.49(13) . . ? N4 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? N4 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C3 N4 C6 122.94(13) . . ? C3 N4 H4 118.5 . . ? C6 N4 H4 118.5 . . ? C8 C7 C5 115.88(14) . . ? C8 C7 H7A 108.3 . . ? C5 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? C5 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C9 C8 C7 111.37(16) . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8B 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C5 116.05(15) . . ? C11 C10 H10A 108.3 . . ? C5 C10 H10A 108.3 . . ? C11 C10 H10B 108.3 . . ? C5 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C10 C11 C12 111.23(18) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? 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 . . ? C15 C13 C14 119.39(15) 2_666 . ? C15 C13 C3 120.54(15) 2_666 . ? C14 C13 C3 120.05(15) . . ? C15 C14 C13 120.48(15) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C13 120.13(15) . 2_666 ? C14 C15 H15 119.9 . . ? C13 C15 H15 119.9 2_666 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.416 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.059 # Attachment 'cationseul982.cif' data_e982a _database_code_depnum_ccdc_archive 'CCDC 790497' #TrackingRef 'cationseul982.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H68 N4, 2(H2 O), 2(Cl)' _chemical_formula_sum 'C38 H72 Cl2 N4 O2' _chemical_formula_weight 687.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2183(7) _cell_length_b 9.5015(7) _cell_length_c 24.6412(18) _cell_angle_alpha 83.832(3) _cell_angle_beta 81.225(2) _cell_angle_gamma 76.505(3) _cell_volume 2068.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2492 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9627 _exptl_absorpt_correction_T_max 0.9718 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 17654 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0841 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.07 _reflns_number_total 8857 _reflns_number_gt 4941 _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^)+(0.0578P)^2^+0.3767P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8857 _refine_ls_number_parameters 425 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1466 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.026 _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 C1 C 0.0412(3) 0.9031(3) 1.09697(10) 0.0236(5) Uani 1 1 d . . . N1 N 0.0193(2) 1.0397(2) 1.10694(8) 0.0249(5) Uani 1 1 d . . . H1 H 0.0691 1.0967 1.0850 0.030 Uiso 1 1 calc R . . C2 C -0.0866(3) 1.0998(3) 1.15398(10) 0.0254(6) Uani 1 1 d . . . H2A H -0.1889 1.1327 1.1430 0.031 Uiso 1 1 calc R . . H2B H -0.0566 1.1850 1.1650 0.031 Uiso 1 1 calc R . . C3 C -0.0891(3) 0.9859(3) 1.20290(10) 0.0229(5) Uani 1 1 d . . . C4 C -0.1246(3) 0.8533(3) 1.18152(10) 0.0258(6) Uani 1 1 d . . . H4A H -0.1100 0.7705 1.2097 0.031 Uiso 1 1 calc R . . H4B H -0.2311 0.8758 1.1749 0.031 Uiso 1 1 calc R . . N2 N -0.0267(2) 0.8129(2) 1.13021(8) 0.0249(5) Uani 1 1 d . . . H2 H -0.0125 0.7232 1.1211 0.030 Uiso 1 1 calc R . . C5 C 0.0650(3) 0.9421(3) 1.22489(10) 0.0243(5) Uani 1 1 d . . . H5A H 0.0619 0.8607 1.2534 0.029 Uiso 1 1 calc R . . H5B H 0.1430 0.9056 1.1943 0.029 Uiso 1 1 calc R . . C6 C 0.1136(3) 1.0619(3) 1.24949(11) 0.0334(6) Uani 1 1 d . . . H6A H 0.0346 1.1019 1.2792 0.040 Uiso 1 1 calc R . . H6B H 0.1235 1.1413 1.2207 0.040 Uiso 1 1 calc R . . C7 C 0.2637(3) 1.0074(3) 1.27291(12) 0.0376(7) Uani 1 1 d . . . H7A H 0.3390 0.9570 1.2442 0.045 Uiso 1 1 calc R . . H7B H 0.2992 1.0926 1.2810 0.045 Uiso 1 1 calc R . . C8 C 0.2584(4) 0.9058(3) 1.32452(12) 0.0441(8) Uani 1 1 d . . . H8A H 0.3628 0.8615 1.3316 0.053 Uiso 1 1 calc R . . H8B H 0.2115 0.8265 1.3179 0.053 Uiso 1 1 calc R . . C9 C 0.1724(4) 0.9771(4) 1.37566(13) 0.0618(10) Uani 1 1 d . . . H9A H 0.0670 1.0189 1.3692 0.074 Uiso 1 1 calc R . . H9B H 0.2174 1.0578 1.3820 0.074 Uiso 1 1 calc R . . C10 C 0.1727(5) 0.8723(5) 1.42725(16) 0.0932(16) Uani 1 1 d . . . H10A H 0.1309 0.7905 1.4209 0.140 Uiso 1 1 calc R . . H10B H 0.1113 0.9230 1.4584 0.140 Uiso 1 1 calc R . . H10C H 0.2761 0.8361 1.4355 0.140 Uiso 1 1 calc R . . C11 C -0.2189(3) 1.0477(3) 1.24729(10) 0.0278(6) Uani 1 1 d . . . H11A H -0.2037 1.1414 1.2567 0.033 Uiso 1 1 calc R . . H11B H -0.3143 1.0680 1.2311 0.033 Uiso 1 1 calc R . . C12 C -0.2365(3) 0.9510(3) 1.30055(11) 0.0349(7) Uani 1 1 d . . . H12A H -0.2538 0.8575 1.2918 0.042 Uiso 1 1 calc R . . H12B H -0.1419 0.9303 1.3172 0.042 Uiso 1 1 calc R . . C13 C -0.3660(3) 1.0204(3) 1.34205(11) 0.0398(7) Uani 1 1 d . . . H13A H -0.4595 1.0431 1.3246 0.048 Uiso 1 1 calc R . . H13B H -0.3473 1.1134 1.3507 0.048 Uiso 1 1 calc R . . C14 C -0.3917(4) 0.9289(4) 1.39580(12) 0.0458(8) Uani 1 1 d . . . H14A H -0.4928 0.9699 1.4150 0.055 Uiso 1 1 calc R . . H14B H -0.3909 0.8294 1.3871 0.055 Uiso 1 1 calc R . . C15 C -0.2770(4) 0.9199(4) 1.43447(14) 0.0622(10) Uani 1 1 d . . . H15A H -0.2769 1.0191 1.4432 0.075 Uiso 1 1 calc R . . H15B H -0.1758 0.8773 1.4157 0.075 Uiso 1 1 calc R . . C16 C -0.3081(5) 0.8283(5) 1.48822(15) 0.0917(16) Uani 1 1 d . . . H16A H -0.4107 0.8660 1.5058 0.138 Uiso 1 1 calc R . . H16B H -0.2361 0.8330 1.5131 0.138 Uiso 1 1 calc R . . H16C H -0.2974 0.7273 1.4802 0.138 Uiso 1 1 calc R . . C17 C 0.1467(3) 0.8449(3) 1.04850(9) 0.0225(5) Uani 1 1 d . . . C18 C 0.2828(3) 0.8889(3) 1.03379(10) 0.0259(6) Uani 1 1 d . . . H18 H 0.3054 0.9607 1.0531 0.031 Uiso 1 1 calc R . . C19 C 0.3844(3) 0.8269(3) 0.99080(10) 0.0257(6) Uani 1 1 d . . . H19 H 0.4769 0.8568 0.9807 0.031 Uiso 1 1 calc R . . C20 C 0.3527(3) 0.7215(3) 0.96237(10) 0.0224(5) Uani 1 1 d . . . C21 C 0.2148(3) 0.6803(3) 0.97661(10) 0.0256(6) Uani 1 1 d . . . H21 H 0.1911 0.6099 0.9569 0.031 Uiso 1 1 calc R . . C22 C 0.1132(3) 0.7419(3) 1.01935(10) 0.0262(6) Uani 1 1 d . . . H22 H 0.0197 0.7136 1.0289 0.031 Uiso 1 1 calc R . . N3 N 0.4908(2) 0.5115(2) 0.91368(8) 0.0255(5) Uani 1 1 d . . . H3 H 0.4391 0.4595 0.9373 0.031 Uiso 1 1 calc R . . C23 C 0.4646(3) 0.6531(3) 0.91756(10) 0.0237(6) Uani 1 1 d . . . C24 C 0.6037(3) 0.4385(3) 0.87101(10) 0.0265(6) Uani 1 1 d . . . H24A H 0.5753 0.3496 0.8627 0.032 Uiso 1 1 calc R . . H24B H 0.7027 0.4093 0.8847 0.032 Uiso 1 1 calc R . . C25 C 0.6159(3) 0.5390(3) 0.81836(10) 0.0237(5) Uani 1 1 d . . . C26 C 0.6460(3) 0.6791(3) 0.83577(10) 0.0246(6) Uani 1 1 d . . . H26A H 0.7489 0.6594 0.8461 0.030 Uiso 1 1 calc R . . H26B H 0.6400 0.7534 0.8043 0.030 Uiso 1 1 calc R . . N4 N 0.5369(2) 0.7352(2) 0.88239(8) 0.0248(5) Uani 1 1 d . . . H4 H 0.5190 0.8285 0.8871 0.030 Uiso 1 1 calc R . . C27 C 0.4686(3) 0.5742(3) 0.79213(10) 0.0253(6) Uani 1 1 d . . . H27A H 0.3855 0.6202 0.8194 0.030 Uiso 1 1 calc R . . H27B H 0.4781 0.6462 0.7604 0.030 Uiso 1 1 calc R . . C28 C 0.4253(3) 0.4441(3) 0.77233(12) 0.0381(7) Uani 1 1 d . . . H28A H 0.3899 0.3838 0.8047 0.046 Uiso 1 1 calc R . . H28B H 0.5156 0.3838 0.7521 0.046 Uiso 1 1 calc R . . C29 C 0.3020(3) 0.4904(3) 0.73474(12) 0.0426(8) Uani 1 1 d . . . H29A H 0.2680 0.4033 0.7279 0.051 Uiso 1 1 calc R . . H29B H 0.2150 0.5565 0.7542 0.051 Uiso 1 1 calc R . . C30 C 0.3502(3) 0.5658(3) 0.67978(12) 0.0410(7) Uani 1 1 d . . . H30A H 0.2605 0.6023 0.6605 0.049 Uiso 1 1 calc R . . H30B H 0.3871 0.6511 0.6869 0.049 Uiso 1 1 calc R . . C31 C 0.4709(5) 0.4735(5) 0.64171(15) 0.0759(9) Uani 1 1 d . . . H31A H 0.4338 0.3893 0.6335 0.091 Uiso 1 1 calc R . . H31B H 0.5608 0.4357 0.6607 0.091 Uiso 1 1 calc R . . C32 C 0.5160(5) 0.5566(5) 0.58772(15) 0.0759(9) Uani 1 1 d . . . H32A H 0.4264 0.5996 0.5698 0.114 Uiso 1 1 calc R . . H32B H 0.5876 0.4898 0.5635 0.114 Uiso 1 1 calc R . . H32C H 0.5632 0.6336 0.5952 0.114 Uiso 1 1 calc R . . C33 C 0.7537(3) 0.4677(3) 0.77897(10) 0.0271(6) Uani 1 1 d . . . H33A H 0.8427 0.4441 0.7989 0.033 Uiso 1 1 calc R . . H33B H 0.7366 0.3751 0.7691 0.033 Uiso 1 1 calc R . . C34 C 0.7899(3) 0.5589(3) 0.72585(11) 0.0343(7) Uani 1 1 d . . . H34A H 0.6969 0.5943 0.7084 0.041 Uiso 1 1 calc R . . H34B H 0.8217 0.6448 0.7353 0.041 Uiso 1 1 calc R . . C35 C 0.9118(3) 0.4793(3) 0.68432(11) 0.0315(6) Uani 1 1 d . . . H35A H 0.8785 0.3959 0.6733 0.038 Uiso 1 1 calc R . . H35B H 1.0040 0.4405 0.7020 0.038 Uiso 1 1 calc R . . C36 C 0.9490(3) 0.5753(3) 0.63313(11) 0.0391(7) Uani 1 1 d . . . H36A H 0.8553 0.6177 0.6167 0.047 Uiso 1 1 calc R . . H36B H 0.9859 0.6563 0.6442 0.047 Uiso 1 1 calc R . . C37 C 1.0654(4) 0.4983(4) 0.58951(12) 0.0465(8) Uani 1 1 d . . . H37A H 1.0266 0.4209 0.5766 0.056 Uiso 1 1 calc R . . H37B H 1.1579 0.4518 0.6061 0.056 Uiso 1 1 calc R . . C38 C 1.1051(4) 0.6006(4) 0.54030(14) 0.0691(12) Uani 1 1 d . . . H38A H 1.0142 0.6461 0.5234 0.104 Uiso 1 1 calc R . . H38B H 1.1799 0.5455 0.5132 0.104 Uiso 1 1 calc R . . H38C H 1.1466 0.6758 0.5526 0.104 Uiso 1 1 calc R . . Cl1 Cl 0.95617(8) 0.48997(7) 0.12248(3) 0.03372(18) Uani 1 1 d . . . Cl2 Cl 0.48632(8) 0.07013(7) 0.87025(3) 0.03565(18) Uani 1 1 d . . . O1 O 0.1780(2) 0.2465(2) 0.05399(8) 0.0348(5) Uani 1 1 d D . . O2 O 0.2933(2) 0.3110(2) 0.94406(8) 0.0336(5) Uani 1 1 d D . . H2C H 0.341(3) 0.239(3) 0.9265(11) 0.045 Uiso 1 1 d D . . H2D H 0.224(3) 0.356(3) 0.9240(11) 0.045 Uiso 1 1 d D . . H1C H 0.129(3) 0.320(2) 0.0678(11) 0.045 Uiso 1 1 d D . . H1D H 0.213(3) 0.263(3) 0.0215(8) 0.045 Uiso 1 1 d 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 C1 0.0261(13) 0.0199(13) 0.0255(13) -0.0006(10) -0.0059(11) -0.0055(11) N1 0.0297(12) 0.0182(11) 0.0253(11) 0.0010(9) 0.0001(9) -0.0053(10) C2 0.0308(14) 0.0177(13) 0.0263(13) -0.0037(10) 0.0012(11) -0.0045(11) C3 0.0249(13) 0.0166(13) 0.0258(13) -0.0035(10) -0.0007(11) -0.0024(11) C4 0.0268(14) 0.0223(14) 0.0278(13) -0.0032(11) 0.0008(11) -0.0068(12) N2 0.0269(11) 0.0207(11) 0.0294(12) -0.0058(9) 0.0003(9) -0.0110(10) C5 0.0276(13) 0.0205(13) 0.0261(13) -0.0018(10) -0.0027(11) -0.0081(11) C6 0.0381(16) 0.0268(15) 0.0401(16) -0.0020(12) -0.0084(13) -0.0148(13) C7 0.0360(16) 0.0352(17) 0.0454(17) -0.0012(14) -0.0115(14) -0.0127(14) C8 0.0501(19) 0.0350(18) 0.054(2) 0.0049(15) -0.0219(16) -0.0162(16) C9 0.065(2) 0.075(3) 0.048(2) 0.0070(19) -0.0104(18) -0.026(2) C10 0.097(4) 0.137(4) 0.058(3) 0.034(3) -0.023(2) -0.061(3) C11 0.0268(14) 0.0249(14) 0.0300(14) -0.0036(11) 0.0004(11) -0.0043(12) C12 0.0394(16) 0.0280(15) 0.0345(15) -0.0052(12) 0.0049(13) -0.0070(14) C13 0.0337(16) 0.0459(19) 0.0367(16) -0.0050(14) 0.0050(13) -0.0081(15) C14 0.0499(19) 0.051(2) 0.0366(17) -0.0085(15) 0.0086(15) -0.0189(17) C15 0.060(2) 0.074(3) 0.049(2) 0.0028(19) -0.0056(18) -0.011(2) C16 0.098(3) 0.099(4) 0.049(2) 0.012(2) 0.006(2) 0.020(3) C17 0.0259(13) 0.0190(13) 0.0236(13) -0.0021(10) -0.0040(11) -0.0062(11) C18 0.0293(14) 0.0210(13) 0.0299(14) -0.0059(11) -0.0033(11) -0.0095(12) C19 0.0255(13) 0.0211(13) 0.0320(14) -0.0020(11) -0.0028(11) -0.0090(11) C20 0.0250(13) 0.0181(13) 0.0249(13) -0.0022(10) -0.0037(11) -0.0062(11) C21 0.0288(14) 0.0233(14) 0.0290(13) -0.0067(11) -0.0044(11) -0.0118(12) C22 0.0241(13) 0.0278(14) 0.0300(14) -0.0057(11) -0.0008(11) -0.0126(12) N3 0.0281(12) 0.0180(11) 0.0283(11) -0.0009(9) 0.0036(9) -0.0061(10) C23 0.0231(13) 0.0220(14) 0.0273(13) -0.0016(11) -0.0040(11) -0.0072(11) C24 0.0280(14) 0.0173(13) 0.0333(14) -0.0021(11) -0.0028(11) -0.0035(11) C25 0.0242(13) 0.0164(13) 0.0292(13) -0.0011(10) -0.0020(11) -0.0033(11) C26 0.0243(13) 0.0202(13) 0.0293(13) -0.0044(10) 0.0005(11) -0.0062(11) N4 0.0267(11) 0.0166(11) 0.0317(11) -0.0051(9) 0.0013(9) -0.0078(9) C27 0.0239(13) 0.0221(14) 0.0300(14) -0.0020(11) -0.0027(11) -0.0059(11) C28 0.0456(18) 0.0318(16) 0.0451(17) 0.0012(13) -0.0159(14) -0.0208(14) C29 0.0417(18) 0.046(2) 0.0479(18) -0.0055(15) -0.0136(15) -0.0191(16) C30 0.0437(18) 0.0397(18) 0.0432(17) -0.0065(14) -0.0160(15) -0.0086(15) C31 0.0690(19) 0.094(2) 0.0626(18) -0.0169(16) 0.0055(15) -0.0172(18) C32 0.0690(19) 0.094(2) 0.0626(18) -0.0169(16) 0.0055(15) -0.0172(18) C33 0.0246(13) 0.0212(14) 0.0339(14) -0.0046(11) 0.0016(11) -0.0038(11) C34 0.0338(15) 0.0275(15) 0.0379(16) -0.0036(12) 0.0039(13) -0.0041(13) C35 0.0272(14) 0.0300(15) 0.0365(15) -0.0059(12) 0.0013(12) -0.0064(12) C36 0.0335(16) 0.0412(18) 0.0400(17) -0.0017(14) 0.0028(13) -0.0088(14) C37 0.0413(18) 0.059(2) 0.0391(17) -0.0094(15) 0.0055(14) -0.0158(17) C38 0.065(2) 0.089(3) 0.045(2) 0.004(2) 0.0158(18) -0.019(2) Cl1 0.0378(4) 0.0215(3) 0.0441(4) -0.0062(3) -0.0054(3) -0.0094(3) Cl2 0.0412(4) 0.0207(4) 0.0470(4) -0.0039(3) -0.0117(3) -0.0064(3) O1 0.0406(12) 0.0259(11) 0.0372(11) -0.0028(9) 0.0000(10) -0.0091(10) O2 0.0347(12) 0.0255(11) 0.0395(12) -0.0035(9) -0.0010(9) -0.0061(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.310(3) . ? C1 N2 1.319(3) . ? C1 C17 1.488(3) . ? N1 C2 1.470(3) . ? N1 H1 0.8800 . ? C2 C3 1.532(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.536(3) . ? C3 C11 1.544(3) . ? C3 C5 1.548(3) . ? C4 N2 1.468(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 H2 0.8800 . ? C5 C6 1.528(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.537(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.514(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.518(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.528(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.529(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.520(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.523(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.510(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.532(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.389(3) . ? C17 C18 1.398(3) . ? C18 C19 1.386(3) . ? C18 H18 0.9500 . ? C19 C20 1.389(3) . ? C19 H19 0.9500 . ? C20 C21 1.400(3) . ? C20 C23 1.483(3) . ? C21 C22 1.380(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? N3 C23 1.322(3) . ? N3 C24 1.469(3) . ? N3 H3 0.8800 . ? C23 N4 1.314(3) . ? C24 C25 1.532(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.538(3) . ? C25 C33 1.542(3) . ? C25 C27 1.544(3) . ? C26 N4 1.464(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? N4 H4 0.8800 . ? C27 C28 1.531(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.531(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.517(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.513(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.525(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.528(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.517(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.519(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.514(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.525(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O1 H1C 0.818(17) . ? O1 H1D 0.830(17) . ? O2 H2C 0.847(17) . ? O2 H2D 0.870(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 N1 C1 N2 121.0(2) . . ? N1 C1 C17 120.7(2) . . ? N2 C1 C17 118.3(2) . . ? C1 N1 C2 121.5(2) . . ? C1 N1 H1 119.3 . . ? C2 N1 H1 119.3 . . ? N1 C2 C3 110.8(2) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 106.4(2) . . ? C2 C3 C11 108.1(2) . . ? C4 C3 C11 108.6(2) . . ? C2 C3 C5 111.2(2) . . ? C4 C3 C5 109.7(2) . . ? C11 C3 C5 112.6(2) . . ? N2 C4 C3 110.8(2) . . ? N2 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C1 N2 C4 123.9(2) . . ? C1 N2 H2 118.0 . . ? C4 N2 H2 118.0 . . ? C6 C5 C3 115.9(2) . . ? C6 C5 H5A 108.3 . . ? C3 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? C3 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 112.5(2) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 115.3(2) . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 C9 114.6(3) . . ? C7 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? C7 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C8 C9 C10 113.2(3) . . ? C8 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C3 115.9(2) . . ? C12 C11 H11A 108.3 . . ? C3 C11 H11A 108.3 . . ? C12 C11 H11B 108.3 . . ? C3 C11 H11B 108.3 . . ? H11A C11 H11B 107.4 . . ? C13 C12 C11 112.5(2) . . ? C13 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? C13 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C12 C13 C14 115.3(3) . . ? C12 C13 H13A 108.4 . . ? C14 C13 H13A 108.4 . . ? C12 C13 H13B 108.4 . . ? C14 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C13 114.5(3) . . ? C15 C14 H14A 108.6 . . ? C13 C14 H14A 108.6 . . ? C15 C14 H14B 108.6 . . ? C13 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C14 C15 C16 112.8(3) . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 119.9(2) . . ? C22 C17 C1 120.1(2) . . ? C18 C17 C1 120.0(2) . . ? C19 C18 C17 119.5(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.8(2) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 119.4(2) . . ? C19 C20 C23 120.1(2) . . ? C21 C20 C23 120.5(2) . . ? C22 C21 C20 120.0(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 120.5(2) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? C23 N3 C24 121.9(2) . . ? C23 N3 H3 119.1 . . ? C24 N3 H3 119.1 . . ? N4 C23 N3 121.1(2) . . ? N4 C23 C20 119.0(2) . . ? N3 C23 C20 120.0(2) . . ? N3 C24 C25 110.8(2) . . ? N3 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C24 C25 C26 106.1(2) . . ? C24 C25 C33 108.5(2) . . ? C26 C25 C33 108.3(2) . . ? C24 C25 C27 111.2(2) . . ? C26 C25 C27 109.7(2) . . ? C33 C25 C27 112.8(2) . . ? N4 C26 C25 111.3(2) . . ? N4 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? N4 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C23 N4 C26 123.2(2) . . ? C23 N4 H4 118.4 . . ? C26 N4 H4 118.4 . . ? C28 C27 C25 115.4(2) . . ? C28 C27 H27A 108.4 . . ? C25 C27 H27A 108.4 . . ? C28 C27 H27B 108.4 . . ? C25 C27 H27B 108.4 . . ? H27A C27 H27B 107.5 . . ? C27 C28 C29 112.3(2) . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C28 114.3(2) . . ? C30 C29 H29A 108.7 . . ? C28 C29 H29A 108.7 . . ? C30 C29 H29B 108.7 . . ? C28 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C31 C30 C29 115.6(3) . . ? C31 C30 H30A 108.4 . . ? C29 C30 H30A 108.4 . . ? C31 C30 H30B 108.4 . . ? C29 C30 H30B 108.4 . . ? H30A C30 H30B 107.4 . . ? C30 C31 C32 112.9(3) . . ? C30 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? C30 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? 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 . . ? C34 C33 C25 115.5(2) . . ? C34 C33 H33A 108.4 . . ? C25 C33 H33A 108.4 . . ? C34 C33 H33B 108.4 . . ? C25 C33 H33B 108.4 . . ? H33A C33 H33B 107.5 . . ? C35 C34 C33 114.5(2) . . ? C35 C34 H34A 108.6 . . ? C33 C34 H34A 108.6 . . ? C35 C34 H34B 108.6 . . ? C33 C34 H34B 108.6 . . ? H34A C34 H34B 107.6 . . ? C34 C35 C36 112.9(2) . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C35 114.6(3) . . ? C37 C36 H36A 108.6 . . ? C35 C36 H36A 108.6 . . ? C37 C36 H36B 108.6 . . ? C35 C36 H36B 108.6 . . ? H36A C36 H36B 107.6 . . ? C36 C37 C38 112.7(3) . . ? C36 C37 H37A 109.1 . . ? C38 C37 H37A 109.1 . . ? C36 C37 H37B 109.1 . . ? C38 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? H1C O1 H1D 112(3) . . ? H2C O2 H2D 105(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.07 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.542 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.055