# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2218 data_PY27AZ _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,7-Diazapyrene ; _chemical_name_common '2.7-diazapyrene' _chemical_melting_point unknown _chemical_formula_moiety 'C14H8N2' _chemical_formula_sum 'C14 H8 N2' _chemical_formula_weight 204.22 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 3.7891(12) _cell_length_b 8.0997(16) _cell_length_c 15.421(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.96(3) _cell_angle_gamma 90.00 _cell_volume 472.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 42 _cell_measurement_theta_min 13.65 _cell_measurement_theta_max 16.7 _exptl_crystal_description column _exptl_crystal_colour yellow/orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 212 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 four-circle' _diffrn_measurement_method 'omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% '+/-5% variation' _diffrn_reflns_number 2590 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0134 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 24.98 _reflns_number_total 839 _reflns_number_gt 673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (Stoe & Cie, 1996a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'X-RED (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-96; PLATON (Spek, 1999)' _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^)+(0.039P)^2^+0.188P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.023(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 839 _refine_ls_number_parameters 78 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.2894(4) 0.1987(2) 0.30144(9) 0.0438(4) Uani 1 1 d . . . C11 C 0.2076(4) 0.0396(2) 0.31246(10) 0.0389(5) Uani 1 1 d . . . H11A H 0.0899 -0.0173 0.2650 0.043(5) Uiso 1 1 calc R . . C12 C 0.2849(4) -0.0484(2) 0.39001(9) 0.0293(4) Uani 1 1 d . . . C13 C 0.4574(4) 0.03973(18) 0.45963(9) 0.0243(4) Uani 1 1 d . . . C16 C 0.1991(4) -0.2186(2) 0.40222(11) 0.0360(4) Uani 1 1 d . . . H16A H 0.0843 -0.2790 0.3556 0.047(5) Uiso 1 1 calc R . . C26 C 0.2787(4) -0.2940(2) 0.47871(11) 0.0346(4) Uani 1 1 d . . . H26A H 0.2176 -0.4068 0.4852 0.047(5) Uiso 1 1 calc R . . C22 C 0.4548(4) -0.20772(19) 0.55115(10) 0.0295(4) Uani 1 1 d . . . C21 C 0.5465(4) -0.2782(2) 0.63194(11) 0.0390(5) Uani 1 1 d . . . H21A H 0.4878 -0.3909 0.6400 0.049(5) 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 N1 0.0393(8) 0.0585(10) 0.0340(8) 0.0121(7) 0.0059(6) 0.0098(7) C11 0.0297(8) 0.0613(12) 0.0253(9) -0.0053(8) -0.0010(7) 0.0076(8) C12 0.0220(7) 0.0393(9) 0.0266(8) -0.0056(7) 0.0017(6) 0.0030(7) C13 0.0185(7) 0.0294(8) 0.0253(7) -0.0029(6) 0.0038(5) 0.0021(6) C16 0.0272(8) 0.0412(10) 0.0393(10) -0.0152(8) 0.0005(7) -0.0028(7) C26 0.0276(8) 0.0257(8) 0.0514(10) -0.0066(8) 0.0081(7) -0.0038(7) C22 0.0237(7) 0.0310(8) 0.0346(9) 0.0035(7) 0.0076(6) 0.0030(6) C21 0.0353(9) 0.0403(10) 0.0425(10) 0.0113(8) 0.0093(7) 0.0054(8) _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 N1 C21 1.330(2) 3_656 ? N1 C11 1.339(2) . ? C11 C12 1.406(2) . ? C12 C13 1.412(2) . ? C12 C16 1.431(2) . ? C13 C22 1.413(2) 3_656 ? C13 C13 1.419(3) 3_656 ? C16 C26 1.344(2) . ? C26 C22 1.442(2) . ? C22 C21 1.392(2) . ? C22 C13 1.413(2) 3_656 ? C21 N1 1.330(2) 3_656 ? 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 C21 N1 C11 117.91(15) 3_656 . ? N1 C11 C12 124.03(16) . . ? C11 C12 C13 116.67(15) . . ? C11 C12 C16 124.36(15) . . ? C13 C12 C16 118.97(14) . . ? C12 C13 C22 119.86(14) . 3_656 ? C12 C13 C13 120.22(17) . 3_656 ? C22 C13 C13 119.91(17) 3_656 3_656 ? C26 C16 C12 120.91(15) . . ? C16 C26 C22 121.58(15) . . ? C21 C22 C13 116.98(15) . 3_656 ? C21 C22 C26 124.62(16) . . ? C13 C22 C26 118.40(14) 3_656 . ? N1 C21 C22 124.55(17) 3_656 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 N1 C11 C12 -0.1(2) 3_656 . . . ? N1 C11 C12 C13 0.5(2) . . . . ? N1 C11 C12 C16 -179.82(15) . . . . ? C11 C12 C13 C22 -0.4(2) . . . 3_656 ? C16 C12 C13 C22 179.84(13) . . . 3_656 ? C11 C12 C13 C13 179.55(16) . . . 3_656 ? C16 C12 C13 C13 -0.2(2) . . . 3_656 ? C11 C12 C16 C26 -179.34(15) . . . . ? C13 C12 C16 C26 0.4(2) . . . . ? C12 C16 C26 C22 -0.4(2) . . . . ? C16 C26 C22 C21 -179.70(15) . . . . ? C16 C26 C22 C13 0.2(2) . . . 3_656 ? C13 C22 C21 N1 -0.3(2) 3_656 . . 3_656 ? C26 C22 C21 N1 179.64(15) . . . 3_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.19 _refine_diff_density_min -0.13 _refine_diff_density_rms 0.03 #===END data_AG27NT _audit_creation_method SHELXL-97 _chemical_name_systematic ; (2,7-Diazapyrene)nitratosilver(I) ; _chemical_name_common [Ag(2,7-diazapyrene)]NO3 _chemical_formula_moiety 'C28 H16 Ag2 N4 2+, 2(N O3 -)' _chemical_formula_sum 'C28 H16 Ag2 N6 O6' _chemical_formula_weight 748.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 18.4700(10) _cell_length_b 3.748(12) _cell_length_c 16.667(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1154(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 1.762 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius FAST TV Detector' _diffrn_measurement_method 'area detector scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3914 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 24.92 _reflns_number_total 904 _reflns_number_gt 688 _reflns_threshold_expression >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction ABSMAD _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 1999)' _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^)+(0.036P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct' _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'placed geometrically' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 904 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.7500 0.2500 0.39235(3) 0.0174(2) Uani 1 2 d S . . N1 N 0.65689(19) 0.5751(10) 0.4332(2) 0.0124(9) Uani 1 1 d . . . C11 C 0.6034(3) 0.6623(11) 0.3813(3) 0.0128(11) Uani 1 1 d . . . H11A H 0.6095 0.6042 0.3262 0.015 Uiso 1 1 calc R . . C12 C 0.5403(2) 0.8310(11) 0.4042(3) 0.0103(11) Uani 1 1 d . . . C13 C 0.5322(2) 0.9152(12) 0.4862(3) 0.0102(10) Uani 1 1 d . . . C16 C 0.4827(2) 0.9217(13) 0.3496(3) 0.0131(10) Uani 1 1 d . . . H16A H 0.4878 0.8665 0.2943 0.016 Uiso 1 1 calc R . . C26 C 0.4214(3) 1.0838(13) 0.3755(3) 0.0132(11) Uani 1 1 d . . . H26A H 0.3840 1.1388 0.3384 0.016 Uiso 1 1 calc R . . C22 C 0.4129(2) 1.1726(11) 0.4585(3) 0.0102(11) Uani 1 1 d . . . C21 C 0.3513(3) 1.3428(12) 0.4888(3) 0.0146(12) Uani 1 1 d . . . H21A H 0.3135 1.4033 0.4525 0.018 Uiso 1 1 calc R . . N10 N 0.7500 0.2500 0.2164(3) 0.0197(13) Uani 1 2 d S . . O1 O 0.69618(19) 0.1334(9) 0.2541(2) 0.0265(9) Uani 1 1 d . . . O2 O 0.7500 0.2500 0.1414(3) 0.0322(13) Uani 1 2 d S . . 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 0.0126(3) 0.0233(3) 0.0164(3) 0.000 0.000 0.0070(2) N1 0.013(2) 0.011(2) 0.013(2) -0.0007(18) 0.0025(18) 0.0012(16) C11 0.014(3) 0.011(3) 0.013(3) 0.0012(18) 0.002(2) -0.0018(19) C12 0.015(2) 0.005(3) 0.012(3) 0.0010(17) 0.003(2) -0.0013(18) C13 0.013(3) 0.003(2) 0.015(3) 0.0013(19) 0.000(2) -0.0021(19) C16 0.020(3) 0.011(2) 0.008(3) 0.0005(19) 0.001(2) -0.001(2) C26 0.012(3) 0.011(2) 0.017(3) 0.001(2) -0.005(2) 0.001(2) C22 0.008(2) 0.012(3) 0.010(2) 0.0005(18) 0.0016(19) -0.0016(18) C21 0.013(3) 0.014(3) 0.017(3) 0.0034(19) -0.005(2) -0.0020(19) N10 0.021(3) 0.022(3) 0.016(3) 0.000 0.000 0.005(3) O1 0.0204(19) 0.041(2) 0.019(2) 0.0045(16) 0.0072(17) -0.0063(17) O2 0.036(3) 0.047(4) 0.014(3) 0.000 0.000 -0.008(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 Ag1 N1 2.215(4) 2_655 y Ag1 O1 2.547(4) . y N1 C21 1.345(6) 5_676 ? N1 C11 1.354(6) . ? C11 C12 1.379(7) . ? C12 C13 1.411(6) . ? C12 C16 1.441(6) . ? C13 C22 1.409(6) 5_676 ? C13 C13 1.424(9) 5_676 ? C16 C26 1.354(7) . ? C26 C22 1.432(6) . ? C22 C21 1.398(7) . ? C22 C13 1.409(6) 5_676 ? C21 N1 1.345(6) 5_676 ? N10 O2 1.249(7) . ? N10 O1 1.255(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 N1 Ag1 N1 144.2(2) 2_655 . y N1 Ag1 O1 119.12(15) 2_655 . y N1 Ag1 O1 93.98(13) . . y O1 Ag1 O1 50.46(16) . 2_655 y C21 N1 C11 118.7(4) 5_676 . ? C21 N1 Ag1 120.7(3) 5_676 . ? C11 N1 Ag1 120.2(3) . . ? N10 O1 Ag1 94.9(3) . . ? N1 C11 C12 123.4(4) . . ? C11 C12 C13 117.5(4) . . ? C11 C12 C16 123.8(4) . . ? C13 C12 C16 118.7(4) . . ? C22 C13 C12 120.3(4) 5_676 . ? C22 C13 C13 119.7(5) 5_676 5_676 ? C12 C13 C13 120.1(5) . 5_676 ? C26 C16 C12 121.5(4) . . ? C16 C26 C22 120.2(4) . . ? C21 C22 C13 117.2(4) . 5_676 ? C21 C22 C26 123.0(4) . . ? C13 C22 C26 119.8(4) 5_676 . ? N1 C21 C22 123.0(4) 5_676 . ? O2 N10 O1 120.1(3) . 2_655 ? O2 N10 O1 120.1(3) . . ? O1 N10 O1 119.8(6) 2_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C21 8.1(3) 2_655 . . 5_676 ? O1 Ag1 N1 C21 166.6(3) . . . 5_676 ? O1 Ag1 N1 C21 -147.1(3) 2_655 . . 5_676 ? N1 Ag1 N1 C11 -164.9(3) 2_655 . . . ? O1 Ag1 N1 C11 -6.4(3) . . . . ? O1 Ag1 N1 C11 39.8(4) 2_655 . . . ? C21 N1 C11 C12 -0.2(6) 5_676 . . . ? Ag1 N1 C11 C12 173.0(3) . . . . ? N1 C11 C12 C13 0.0(7) . . . . ? N1 C11 C12 C16 -179.3(4) . . . . ? C11 C12 C13 C22 0.0(6) . . . 5_676 ? C16 C12 C13 C22 179.4(4) . . . 5_676 ? C11 C12 C13 C13 -179.1(5) . . . 5_676 ? C16 C12 C13 C13 0.3(7) . . . 5_676 ? C11 C12 C16 C26 179.2(4) . . . . ? C13 C12 C16 C26 -0.1(7) . . . . ? C12 C16 C26 C22 0.6(7) . . . . ? C16 C26 C22 C21 179.4(4) . . . . ? C16 C26 C22 C13 -1.2(7) . . . 5_676 ? C13 C22 C21 N1 0.3(7) 5_676 . . 5_676 ? C26 C22 C21 N1 179.7(4) . . . 5_676 ? O2 N10 O1 Ag1 180.0 . . . . ? O1 N10 O1 Ag1 0.0 2_655 . . . ? N1 Ag1 O1 N10 -69.1(3) 2_655 . . . ? N1 Ag1 O1 N10 125.1(2) . . . . ? O1 Ag1 O1 N10 0.0 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 24.92 _diffrn_measured_fraction_theta_full 0.889 _refine_diff_density_max 0.57 _refine_diff_density_min -0.66 _refine_diff_density_rms 0.14 #===END data_agacpy _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{Ag[1,4-bis(4-pyridyl)butadiyne]tetrafluoroborate}.acetonitrile solvate' ; _chemical_name_common {[Ag(pybut)]BF4.MeCN}n _chemical_formula_moiety {[Ag(pybut)]BF4.MeCN}n _chemical_formula_sum 'C16 H11 Ag B F4 N3' _chemical_formula_weight 439.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 8.175(3) _cell_length_b 7.147(2) _cell_length_c 14.917(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.28(3) _cell_angle_gamma 90.00 _cell_volume 871.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14.0 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 0.833 _exptl_special_details ; '{Ag[1,4-bis(4-pyridyl)butadiyne]tetrafluoroborate}.acetonitrile solvate' ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE STADI-4 FOUR-CIRCLE DIFFRACTOMETER D092' _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'non-linear 7.2% decay' _diffrn_reflns_number 2352 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 24.95 _reflns_number_total 1534 _reflns_number_gt 1221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (stoe & cie, 1996a)' _computing_cell_refinement 'STADI-4 (stoe & cie, 1996a)' _computing_data_reduction 'X-RED (stoe & cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (version 5.03)(Sheldrick,1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.055P)^2^+1.439P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct method' _atom_sites_solution_secondary 'difference Fourier method' _atom_sites_solution_hydrogens 'aromatic placed geometrically, Me-group not found' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1534 _refine_ls_number_parameters 113 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.054 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.5000 0.5000 0.0615(3) Uani 1 d S . . N1 N 0.1337(5) 0.2414(5) 0.4995(3) 0.0511(10) Uani 1 d . . . C4 C 0.2689(8) 0.0011(6) 0.4209(4) 0.0589(14) Uani 1 d . . . H4A H 0.3047 -0.0452 0.3665 0.071 Uiso 1 calc R . . C1 C 0.4568(7) -0.4188(7) 0.5001(4) 0.0584(13) Uani 1 d . . . C2 C 0.3821(6) -0.2733(7) 0.4993(4) 0.0548(12) Uani 1 d . . . C3 C 0.2970(6) -0.0987(6) 0.4988(4) 0.0493(11) Uani 1 d . . . C6 C 0.1601(7) 0.1455(8) 0.5734(4) 0.0649(15) Uani 1 d . . . H6A H 0.1218 0.1947 0.6267 0.078 Uiso 1 calc R . . C7 C 0.2404(8) -0.0222(7) 0.5770(4) 0.0638(15) Uani 1 d . . . H7A H 0.2565 -0.0837 0.6314 0.077 Uiso 1 calc R . . C5 C 0.1884(7) 0.1681(8) 0.4241(4) 0.0657(15) Uani 1 d . . . H5A H 0.1709 0.2337 0.3709 0.079 Uiso 1 calc R . . B1 B 0.0000 0.4909(12) 0.7500 0.057(2) Uani 1 d S . . F1 F 0.0962(6) 0.5937(8) 0.6966(3) 0.1209(18) Uani 1 d . . . F2 F -0.0928(11) 0.3525(13) 0.7129(6) 0.086(3) Uiso 0.50 d P A 1 F2' F -0.1063(9) 0.4122(12) 0.6828(5) 0.0692(19) Uiso 0.50 d P A 2 N1S N -0.5000 0.414(4) 0.7500 0.163(16) Uiso 0.50 d SPD B 1 C1S C -0.5000 0.578(4) 0.7500 0.084(6) Uiso 0.50 d SPD B 1 C2S C -0.5000 0.778(4) 0.7500 0.075(6) Uiso 0.50 d SPD B 1 N1S' N -0.5000 0.836(3) 0.7500 0.098(9) Uiso 0.50 d SPD C 2 C1S' C -0.5000 0.673(3) 0.7500 0.044(3) Uiso 0.50 d SPD C 2 C2S' C -0.5000 0.463(3) 0.7500 0.077(7) Uiso 0.50 d SPD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0615(4) 0.0324(3) 0.0907(5) -0.0009(3) 0.0016(3) 0.0202(2) N1 0.047(2) 0.0317(19) 0.074(3) 0.0010(19) 0.0021(19) 0.0147(16) C4 0.076(4) 0.041(3) 0.059(3) -0.003(2) 0.010(3) 0.024(2) C1 0.061(3) 0.037(3) 0.077(4) -0.001(2) 0.000(3) 0.004(2) C2 0.058(3) 0.039(2) 0.067(3) -0.001(2) 0.002(2) 0.013(2) C3 0.045(2) 0.029(2) 0.073(3) -0.001(2) 0.003(2) 0.0064(18) C6 0.074(4) 0.050(3) 0.071(4) -0.001(3) 0.009(3) 0.027(3) C7 0.074(4) 0.050(3) 0.068(4) 0.011(3) 0.007(3) 0.025(3) C5 0.073(4) 0.056(3) 0.069(4) 0.007(3) 0.004(3) 0.027(3) B1 0.054(5) 0.054(5) 0.062(5) 0.000 0.003(4) 0.000 F1 0.105(3) 0.134(4) 0.124(4) 0.068(3) -0.006(3) -0.025(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 Ag1 N1 2.147(3) . y Ag1 N1 2.147(3) 3_566 ? N1 C6 1.312(7) . ? N1 C5 1.327(7) . ? C4 C5 1.365(7) . ? C4 C3 1.378(7) . ? C1 C2 1.206(7) . y C1 C1 1.359(11) 3_646 y C2 C3 1.429(6) . y C3 C7 1.377(8) . ? C6 C7 1.367(7) . ? B1 F1 1.349(6) . ? B1 F1 1.349(6) 2_556 ? B1 F2 1.357(10) . ? B1 F2 1.357(10) 2_556 ? B1 F2' 1.428(8) . ? B1 F2' 1.428(8) 2_556 ? N1S C1S 1.174(18) . ? C1S C2S 1.432(17) . ? N1S' C1S' 1.166(17) . ? C1S' C2S' 1.499(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 Ag1 N1 180.000(1) . 3_566 y C6 N1 C5 117.0(4) . . ? C6 N1 Ag1 121.4(3) . . ? C5 N1 Ag1 121.6(3) . . ? C5 C4 C3 119.6(5) . . ? C2 C1 C1 178.9(8) . 3_646 ? C1 C2 C3 178.7(6) . . ? C7 C3 C4 117.1(4) . . ? C7 C3 C2 121.0(5) . . ? C4 C3 C2 121.9(5) . . ? N1 C6 C7 124.1(5) . . ? C6 C7 C3 119.0(5) . . ? N1 C5 C4 123.1(5) . . ? F1 B1 F1 114.0(8) . 2_556 ? F1 B1 F2 119.0(5) . . ? F1 B1 F2 108.0(5) 2_556 . ? F1 B1 F2 108.0(5) . 2_556 ? F1 B1 F2 119.0(5) 2_556 2_556 ? F2 B1 F2 86.4(10) . 2_556 ? F1 B1 F2' 98.9(4) . . ? F1 B1 F2' 106.0(4) 2_556 . ? F1 B1 F2' 106.0(4) . 2_556 ? F1 B1 F2' 98.9(4) 2_556 2_556 ? F2' B1 F2' 133.5(10) . 2_556 ? N1S C1S C2S 180.00(3) . . ? N1S' C1S' C2S' 180.00(2) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 0.560 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.087 #===END data_ag4bpy _audit_creation_method SHELXL-97 _chemical_name_systematic ; 4,4'-Bipyridyl silver tetraflouroborate complex monohydrate acetonitrile solvate ; _chemical_name_common '4,4-Bipy*AgBF4*H2O ' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C10 H8 N2 Ag +, B F4 -, H2 O, C2 H3 N' _chemical_formula_sum 'C12 H13 Ag B F4 N3 O' _chemical_formula_weight 409.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.273(2) _cell_length_b 10.506(3) _cell_length_c 10.642(3) _cell_angle_alpha 96.33(4) _cell_angle_beta 103.29(3) _cell_angle_gamma 98.16(3) _cell_volume 774.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14.0 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 1.345 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 'Stadi-4' _diffrn_measurement_method 'omega/theta' # PLEASE CHECK _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'variations +-5.3' _diffrn_reflns_number 3981 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2730 _reflns_number_gt 2153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (Stoe & Cie, 1996a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'X-RED (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-96; PLATON (Spek, 1999)' _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^)+(0.070P)^2^+5.348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct method' _atom_sites_solution_secondary 'difference Fourier method' _atom_sites_solution_hydrogens 'Me-group from delta-F synthesis, others placed geometrically' _refine_ls_hydrogen_treatment 'rigid rotator for Me-group, riding model for others' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2730 _refine_ls_number_parameters 208 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1527 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.118 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -1.03574(10) -0.08993(8) -0.27541(6) 0.0485(3) Uani 1 1 d . . . N1 N -0.8327(9) -0.0948(7) -0.0919(6) 0.0372(15) Uani 1 1 d . . . N1S N -0.0321(12) -0.1786(9) 0.2407(8) 0.056(2) Uani 1 1 d . . . N2 N -0.2405(9) -0.0956(7) 0.5385(6) 0.0377(16) Uani 1 1 d . . . C1 C -0.5984(10) -0.0973(7) 0.1567(7) 0.0292(16) Uani 1 1 d . . . C1S C -0.0727(14) -0.2848(10) 0.2047(9) 0.049(2) Uani 1 1 d . . . C2 C -0.6544(11) 0.0173(8) 0.1193(7) 0.0327(17) Uani 1 1 d . . . H2A H -0.6148 0.0956 0.1777 0.039 Uiso 1 1 calc R . . C2S C -0.127(2) -0.4240(12) 0.1563(13) 0.097(5) Uani 1 1 d . . . H2SA H -0.0128 -0.4641 0.1709 0.146 Uiso 1 1 calc R . . H2SA H -0.1876 -0.4369 0.0636 0.146 Uiso 1 1 calc R . . H2SA H -0.2153 -0.4634 0.2023 0.146 Uiso 1 1 calc R . . C3 C -0.7684(11) 0.0145(8) -0.0038(7) 0.0331(17) Uani 1 1 d . . . H3A H -0.8035 0.0928 -0.0280 0.040 Uiso 1 1 calc R . . C4 C -0.7751(12) -0.2034(8) -0.0561(8) 0.0402(19) Uani 1 1 d . . . H4A H -0.8153 -0.2802 -0.1168 0.048 Uiso 1 1 calc R . . C5 C -0.6596(12) -0.2095(8) 0.0651(8) 0.0388(19) Uani 1 1 d . . . H5A H -0.6229 -0.2885 0.0855 0.047 Uiso 1 1 calc R . . C6 C -0.4763(11) -0.0953(8) 0.2895(7) 0.0324(17) Uani 1 1 d . . . C7 C -0.3600(11) 0.0168(8) 0.3623(7) 0.0339(17) Uani 1 1 d . . . H7A H -0.3590 0.0960 0.3289 0.041 Uiso 1 1 calc R . . C8 C -0.2460(11) 0.0121(8) 0.4835(7) 0.0368(18) Uani 1 1 d . . . H8A H -0.1674 0.0894 0.5304 0.044 Uiso 1 1 calc R . . C9 C -0.3537(12) -0.2064(8) 0.4701(8) 0.042(2) Uani 1 1 d . . . H9A H -0.3531 -0.2836 0.5071 0.050 Uiso 1 1 calc R . . C10 C -0.4700(12) -0.2089(8) 0.3476(7) 0.0373(18) Uani 1 1 d . . . H10A H -0.5462 -0.2877 0.3021 0.045 Uiso 1 1 calc R . . O1 O -0.9389(15) -0.3704(13) -0.4549(10) 0.108(3) Uani 1 1 d D . . H1WB H -0.895(7) -0.311(4) -0.383(4) 0.004(15) Uiso 1 1 d D . . H1WA H -0.853(9) -0.424(7) -0.456(7) 0.06(3) Uiso 1 1 d D . . B1 B -0.6385(17) 0.3950(10) 0.2140(11) 0.070(4) Uani 1 1 d D . . F1 F -0.4972(18) 0.3290(13) 0.2646(13) 0.120(6) Uiso 0.71(2) 1 d PD A 1 F1' F -0.522(5) 0.459(3) 0.330(2) 0.135(17) Uiso 0.29(2) 1 d PD A 2 F2 F -0.565(3) 0.4940(15) 0.1578(16) 0.102(8) Uiso 0.50(3) 1 d PD A 1 F2' F -0.685(3) 0.5086(13) 0.1763(18) 0.108(8) Uiso 0.50(3) 1 d PD A 2 F3 F -0.774(2) 0.3046(15) 0.1255(15) 0.127(8) Uiso 0.61(3) 1 d PD A 1 F3' F -0.594(6) 0.344(4) 0.103(2) 0.177(18) Uiso 0.39(3) 1 d PD A 2 F4 F -0.665(5) 0.460(3) 0.325(2) 0.114(13) Uiso 0.33(3) 1 d PD A 1 F4' F -0.795(3) 0.343(2) 0.253(2) 0.185(11) Uiso 0.67(3) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0435(4) 0.0673(5) 0.0273(4) 0.0119(3) -0.0083(3) 0.0101(3) N1 0.035(4) 0.045(4) 0.028(3) 0.009(3) -0.001(3) 0.007(3) N1S 0.063(5) 0.049(5) 0.047(5) 0.006(4) -0.002(4) 0.005(4) N2 0.035(4) 0.048(4) 0.024(3) 0.005(3) -0.005(3) 0.007(3) C1 0.024(3) 0.036(4) 0.027(4) 0.006(3) 0.003(3) 0.005(3) C1S 0.055(6) 0.053(6) 0.037(5) 0.010(4) 0.006(4) 0.005(5) C2 0.034(4) 0.034(4) 0.027(4) 0.001(3) 0.004(3) 0.007(3) C2S 0.139(13) 0.050(7) 0.080(9) -0.004(6) -0.001(9) -0.003(8) C3 0.034(4) 0.033(4) 0.030(4) 0.011(3) 0.001(3) 0.005(3) C4 0.044(5) 0.039(5) 0.030(4) 0.002(3) -0.003(3) 0.004(4) C5 0.047(5) 0.030(4) 0.036(4) 0.009(3) 0.000(4) 0.007(4) C6 0.033(4) 0.038(4) 0.024(4) 0.004(3) 0.001(3) 0.011(3) C7 0.036(4) 0.034(4) 0.028(4) 0.005(3) 0.001(3) 0.005(3) C8 0.038(4) 0.040(5) 0.029(4) 0.003(3) 0.005(3) 0.002(4) C9 0.048(5) 0.041(5) 0.037(4) 0.017(4) 0.001(4) 0.015(4) C10 0.042(4) 0.034(4) 0.031(4) 0.006(3) 0.000(3) 0.007(4) O1 0.092(7) 0.151(10) 0.078(7) 0.037(7) -0.008(5) 0.047(7) B1 0.096(10) 0.062(8) 0.063(8) 0.016(6) 0.027(7) 0.029(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.171(6) . y Ag1 N2 2.176(6) 1_454 y N1 C4 1.335(10) . ? N1 C3 1.351(10) . ? N1S C1S 1.113(12) . ? N2 C8 1.331(10) . ? N2 C9 1.353(11) . ? N2 Ag1 2.176(6) 1_656 ? C1 C5 1.391(11) . ? C1 C2 1.394(10) . ? C1 C6 1.482(9) . ? C1S C2S 1.461(15) . ? C2 C3 1.375(10) . ? C4 C5 1.381(11) . ? C6 C7 1.385(11) . ? C6 C10 1.405(11) . ? C7 C8 1.374(10) . ? C9 C10 1.377(11) . ? B1 F2 1.360(8) . ? B1 F4' 1.361(8) . ? B1 F1 1.363(8) . ? B1 F2' 1.363(8) . ? B1 F3' 1.368(9) . ? B1 F3 1.368(8) . ? B1 F1' 1.368(9) . ? B1 F4 1.370(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 N1 Ag1 N2 177.1(3) . 1_454 y C4 N1 C3 116.8(6) . . ? C4 N1 Ag1 123.4(5) . . ? C3 N1 Ag1 119.7(5) . . ? C8 N2 C9 117.6(6) . . ? C8 N2 Ag1 119.2(5) . 1_656 ? C9 N2 Ag1 122.9(5) . 1_656 ? C5 C1 C2 117.5(6) . . ? C5 C1 C6 122.8(7) . . ? C2 C1 C6 119.6(7) . . ? N1S C1S C2S 179.5(11) . . ? C3 C2 C1 119.3(7) . . ? N1 C3 C2 123.4(7) . . ? N1 C4 C5 123.7(8) . . ? C4 C5 C1 119.2(7) . . ? C7 C6 C10 116.2(7) . . ? C7 C6 C1 122.4(7) . . ? C10 C6 C1 121.3(7) . . ? C8 C7 C6 119.9(7) . . ? N2 C8 C7 123.8(7) . . ? N2 C9 C10 121.6(7) . . ? C9 C10 C6 120.9(8) . . ? F2 B1 F4' 144.5(15) . . ? F2 B1 F1 109.8(13) . . ? F4' B1 F1 105.1(13) . . ? F2 B1 F2' 41.6(9) . . ? F4' B1 F2' 103.2(15) . . ? F1 B1 F2' 147.4(14) . . ? F2 B1 F3' 71.2(18) . . ? F4' B1 F3' 123(2) . . ? F1 B1 F3' 78.8(17) . . ? F2' B1 F3' 99.0(19) . . ? F2 B1 F3 112.4(13) . . ? F4' B1 F3 62.6(12) . . ? F1 B1 F3 105.3(11) . . ? F2' B1 F3 101.8(12) . . ? F3' B1 F3 61.6(17) . . ? F2 B1 F1' 86.7(19) . . ? F4' B1 F1' 101(2) . . ? F1 B1 F1' 67.5(18) . . ? F2' B1 F1' 91.5(19) . . ? F3' B1 F1' 130(3) . . ? F3 B1 F1' 161(2) . . ? F2 B1 F4 102.0(16) . . ? F4' B1 F4 64.6(15) . . ? F1 B1 F4 101.1(16) . . ? F2' B1 F4 76.9(16) . . ? F3' B1 F4 172(2) . . ? F3 B1 F4 125.2(17) . . ? F1' B1 F4 44.4(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.082 _refine_diff_density_min -0.798 _refine_diff_density_rms 0.133 #===END data_agacby _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-bis(4'-Bipyridyl)buta-1,3-diyne silver nitrate complex acetonitrile sollvate ; _chemical_name_common 'AgNO3*Pubut' _chemical_melting_point unknown _chemical_formula_moiety 'C14 H8 N2 Ag+, N O3-, C2 H3 N' _chemical_formula_sum 'C16 H11 Ag N4 O3' _chemical_formula_weight 415.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 7.134(2) _cell_length_b 7.322(2) _cell_length_c 31.725(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.53(2) _cell_angle_gamma 90.00 _cell_volume 1642.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description 'irregular plate' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stadi-4' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'random variation +-6.3%' _diffrn_reflns_number 3211 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 26.02 _reflns_number_total 3211 _reflns_number_gt 2446 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.15P)^2^+14.00P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct method' _atom_sites_solution_secondary 'difference Fourier synthesis' _atom_sites_solution_hydrogens 'aromatic placed geometrically, others from delta-F synthesis' _refine_ls_hydrogen_treatment 'riding model for aromatic, rigid rotator for Me-groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3211 _refine_ls_number_parameters 216 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.2645 _refine_ls_wR_factor_gt 0.2331 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.006 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.09653(9) 0.03115(13) -0.077501(18) 0.0544(4) Uani 1 1 d U . . N1 N -0.0342(9) 0.0216(10) -0.1430(2) 0.0381(16) Uani 1 1 d U . . N2 N -0.7838(10) -0.0168(10) -0.5117(2) 0.0381(16) Uani 1 1 d U . . C1 C -0.3613(11) 0.0102(11) -0.3071(3) 0.0327(17) Uani 1 1 d U . . C2 C -0.2897(10) 0.0075(11) -0.2699(2) 0.0319(17) Uani 1 1 d U . . C3 C -0.2025(11) 0.0160(11) -0.2274(2) 0.0331(16) Uani 1 1 d U . . C4 C -0.1574(11) -0.1443(13) -0.2049(2) 0.0392(17) Uani 1 1 d U . . H4A H -0.1826 -0.2597 -0.2181 0.047 Uiso 1 1 calc R . . C5 C -0.0753(11) -0.1335(13) -0.1629(2) 0.0403(18) Uani 1 1 d U . . H5A H -0.0473 -0.2441 -0.1477 0.048 Uiso 1 1 calc R . . C6 C -0.0746(12) 0.1768(14) -0.1647(3) 0.0438(19) Uani 1 1 d U . . H6A H -0.0439 0.2895 -0.1507 0.053 Uiso 1 1 calc R . . C7 C -0.1587(12) 0.1811(13) -0.2065(2) 0.0418(18) Uani 1 1 d U . . H7A H -0.1861 0.2942 -0.2206 0.050 Uiso 1 1 calc R . . C8 C -0.4445(11) 0.0056(11) -0.3482(2) 0.0318(17) Uani 1 1 d U . . C9 C -0.5199(11) 0.0000(11) -0.3842(3) 0.0336(17) Uani 1 1 d U . . C10 C -0.6123(10) -0.0058(11) -0.4272(2) 0.0316(16) Uani 1 1 d U . . C11 C -0.6791(14) -0.1659(14) -0.4460(3) 0.053(2) Uani 1 1 d U . . H11A H -0.6667 -0.2760 -0.4300 0.063 Uiso 1 1 calc R . . C12 C -0.7639(14) -0.1694(14) -0.4876(3) 0.053(2) Uani 1 1 d U . . H12A H -0.8097 -0.2822 -0.4996 0.063 Uiso 1 1 calc R . . C13 C -0.7225(14) 0.1381(14) -0.4934(3) 0.051(2) Uani 1 1 d U . . H13A H -0.7368 0.2473 -0.5097 0.061 Uiso 1 1 calc R . . C14 C -0.6379(14) 0.1484(14) -0.4515(3) 0.051(2) Uani 1 1 d U . . H14A H -0.5978 0.2632 -0.4396 0.061 Uiso 1 1 calc R . . N10 N 0.1360(13) -0.4971(9) -0.08122(19) 0.070(3) Uani 1 1 d DU . . O1 O 0.2405(13) -0.6313(11) -0.0819(3) 0.086(3) Uani 1 1 d DU . . O2 O 0.1943(17) -0.3406(11) -0.0854(3) 0.110(4) Uani 1 1 d DU . . O3 O -0.0298(18) -0.5228(18) -0.0765(6) 0.180(9) Uani 1 1 d DU . . N1S N 0.3803(18) 0.5014(17) 0.1385(4) 0.032(3) Uiso 0.50 1 d PDU A -1 C1S C 0.467(6) 0.489(6) 0.1721(7) 0.122(15) Uiso 0.50 1 d PDU A -1 C2S C 0.562(2) 0.485(2) 0.2167(4) 0.033(3) Uiso 0.50 1 d PDU A -1 H2SA H 0.6982 0.4702 0.2169 0.050 Uiso 0.50 1 calc PR A -1 H2SB H 0.5119 0.3829 0.2318 0.050 Uiso 0.50 1 calc PR A -1 H2SC H 0.5366 0.6000 0.2309 0.050 Uiso 0.50 1 calc PR A -1 N1S' N 0.8275(17) 0.4817(17) 0.2052(4) 0.033(3) Uiso 0.50 1 d PDU B -2 C1S' C 0.680(3) 0.486(4) 0.1877(8) 0.077(7) Uiso 0.50 1 d PDU B -2 C2S' C 0.513(3) 0.491(4) 0.1565(8) 0.065(6) Uiso 0.50 1 d PDU B -2 H2SD H 0.4011 0.4631 0.1704 0.098 Uiso 0.50 1 calc PR B -2 H2SE H 0.5243 0.4016 0.1341 0.098 Uiso 0.50 1 calc PR B -2 H2SF H 0.4991 0.6139 0.1440 0.098 Uiso 0.50 1 calc PR B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0331(5) 0.1122(8) 0.0146(4) 0.0005(3) -0.0096(3) -0.0011(3) N1 0.025(3) 0.076(5) 0.011(3) -0.002(3) -0.005(2) -0.001(3) N2 0.029(3) 0.070(5) 0.013(3) 0.000(3) -0.006(2) 0.001(3) C1 0.026(4) 0.048(5) 0.021(3) -0.003(3) -0.005(3) -0.001(3) C2 0.019(3) 0.059(5) 0.017(3) -0.003(3) -0.001(3) 0.001(3) C3 0.023(3) 0.061(5) 0.014(3) 0.000(3) -0.002(3) 0.001(3) C4 0.034(4) 0.058(5) 0.023(3) -0.002(3) -0.006(3) -0.005(4) C5 0.035(4) 0.060(5) 0.023(3) 0.008(3) -0.007(3) -0.008(4) C6 0.044(4) 0.062(5) 0.021(3) -0.005(3) -0.009(3) 0.010(4) C7 0.043(4) 0.057(5) 0.022(3) -0.001(3) -0.008(3) 0.005(4) C8 0.025(4) 0.053(5) 0.018(3) 0.000(3) 0.002(3) -0.002(3) C9 0.027(4) 0.046(5) 0.025(4) 0.000(3) -0.006(3) -0.003(3) C10 0.022(3) 0.057(5) 0.014(3) 0.000(3) -0.004(3) 0.000(3) C11 0.073(6) 0.048(5) 0.030(4) 0.002(3) -0.019(4) 0.004(5) C12 0.070(6) 0.049(5) 0.033(4) -0.009(4) -0.021(4) 0.000(5) C13 0.063(6) 0.056(5) 0.026(4) 0.012(4) -0.021(4) -0.007(5) C14 0.062(6) 0.055(5) 0.028(4) 0.001(3) -0.019(4) -0.012(4) N10 0.095(6) 0.061(5) 0.045(5) -0.005(4) -0.025(5) 0.010(4) O1 0.104(6) 0.054(5) 0.097(7) 0.012(5) -0.001(5) 0.015(4) O2 0.219(11) 0.044(4) 0.055(5) 0.003(4) -0.034(6) -0.006(6) O3 0.122(10) 0.168(13) 0.26(2) -0.071(13) 0.082(14) 0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.153(7) 4_656 y Ag1 N1 2.164(6) . y N1 C5 1.314(12) . ? N1 C6 1.341(12) . ? N2 C13 1.322(12) . ? N2 C12 1.351(12) . ? N2 Ag1 2.152(7) 4_455 ? C1 C2 1.224(12) . ? C1 C8 1.359(13) . ? C2 C3 1.410(11) . ? C3 C4 1.390(12) . ? C3 C7 1.395(12) . ? C4 C5 1.385(10) . ? C6 C7 1.380(10) . ? C8 C9 1.199(12) . ? C9 C10 1.435(11) . ? C10 C14 1.365(12) . ? C10 C11 1.371(13) . ? C11 C12 1.378(11) . ? C13 C14 1.389(11) . ? N10 O3 1.227(9) . ? N10 O2 1.231(8) . ? N10 O1 1.235(8) . ? N1S C1S 1.164(9) . ? C1S C2S 1.486(9) . ? N1S' C1S' 1.124(9) . ? C1S' C2S' 1.448(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 Ag1 N1 174.9(3) 4_656 . y C5 N1 C6 117.7(7) . . ? C5 N1 Ag1 122.0(6) . . ? C6 N1 Ag1 120.2(6) . . ? C13 N2 C12 117.2(7) . . ? C13 N2 Ag1 122.3(6) . 4_455 ? C12 N2 Ag1 120.5(6) . 4_455 ? C2 C1 C8 177.4(9) . . ? C1 C2 C3 176.2(9) . . ? C4 C3 C7 117.7(7) . . ? C4 C3 C2 119.9(7) . . ? C7 C3 C2 122.5(7) . . ? C5 C4 C3 119.1(8) . . ? N1 C5 C4 123.4(8) . . ? N1 C6 C7 123.4(9) . . ? C6 C7 C3 118.6(8) . . ? C9 C8 C1 179.0(9) . . ? C8 C9 C10 179.3(9) . . ? C14 C10 C11 116.7(7) . . ? C14 C10 C9 121.5(7) . . ? C11 C10 C9 121.8(7) . . ? C10 C11 C12 121.0(9) . . ? N2 C12 C11 121.8(9) . . ? N2 C13 C14 122.9(8) . . ? C10 C14 C13 120.3(9) . . ? O3 N10 O2 120.0(9) . . ? O3 N10 O1 118.3(8) . . ? O2 N10 O1 121.7(9) . . ? N1S C1S C2S 174(4) . . ? N1S' C1S' C2S' 167(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.163 _refine_diff_density_min -2.586 _refine_diff_density_rms 0.202 #===END data_AGDYNE _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,4-Bis(4'-pyridyl)butadiynesilver(I)] bis(difluorodioxophosphate) acetonitrile solvate ; _chemical_name_common '[agdbp]PO2F2' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C14 H8 N2 Ag +, P O2 F2 -, C2 H3 N' _chemical_formula_sum 'C16 H11 Ag F2 N3 O2 P' _chemical_formula_weight 454.12 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4930(15) _cell_length_b 8.2850(17) _cell_length_c 14.723(3) _cell_angle_alpha 101.91(3) _cell_angle_beta 90.11(3) _cell_angle_gamma 107.69(3) _cell_volume 850.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 17.5 _exptl_crystal_description lozenge _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 1.315 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.672 _exptl_absorpt_correction_T_max 0.822 _exptl_absorpt_process_details 'North, Phillips & Mathews, 1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe Stadi-4 four-circle' _diffrn_measurement_method 'omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 'variation +/-5' _diffrn_reflns_number 4703 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.16 _reflns_number_total 3005 _reflns_number_gt 2701 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI-4 (Stoe & Cie, 1996a)' _computing_cell_refinement STADI-4 _computing_data_reduction 'X-RED (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material SHELXL-96; PLATON (Spek, 1999)' _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^)+(0.036P)^2^+1.048P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'methyl group from delta-F synthesis, others placed geometrically' _refine_ls_hydrogen_treatment 'rigid rotator for methyl group, riding model for others' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression ? _refine_ls_number_reflns 3005 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.34733(4) 0.56071(4) 0.452256(17) 0.02398(12) Uani 1 1 d . . . N1 N 0.4665(4) 0.5583(4) 0.31681(18) 0.0200(6) Uani 1 1 d . . . C6 C 0.5254(5) 0.7049(5) 0.2853(2) 0.0252(8) Uani 1 1 d . . . H6A H 0.5110 0.8058 0.3214 0.030 Uiso 1 1 calc R . . C7 C 0.6064(5) 0.7126(5) 0.2018(2) 0.0266(8) Uani 1 1 d . . . H7A H 0.6460 0.8169 0.1822 0.032 Uiso 1 1 calc R . . C3 C 0.6282(5) 0.5619(5) 0.1471(2) 0.0203(7) Uani 1 1 d . . . C4 C 0.5662(5) 0.4088(5) 0.1792(2) 0.0210(7) Uani 1 1 d . . . H4A H 0.5785 0.3060 0.1444 0.025 Uiso 1 1 calc R . . C5 C 0.4859(5) 0.4125(5) 0.2637(2) 0.0206(7) Uani 1 1 d . . . H5A H 0.4435 0.3099 0.2847 0.025 Uiso 1 1 calc R . . N2 N 0.1862(4) 0.5703(4) 0.57576(18) 0.0197(6) Uani 1 1 d . . . C13 C 0.1783(5) 0.7197(5) 0.6287(2) 0.0241(8) Uani 1 1 d . . . H13A H 0.2329 0.8218 0.6086 0.029 Uiso 1 1 calc R . . C14 C 0.0927(5) 0.7297(5) 0.7120(2) 0.0246(8) Uani 1 1 d . . . H14A H 0.0901 0.8360 0.7470 0.030 Uiso 1 1 calc R . . C10 C 0.0103(5) 0.5763(5) 0.7423(2) 0.0195(7) Uani 1 1 d . . . C11 C 0.0144(5) 0.4205(5) 0.6858(2) 0.0218(7) Uani 1 1 d . . . H11A H -0.0424 0.3160 0.7032 0.026 Uiso 1 1 calc R . . C12 C 0.1034(5) 0.4227(5) 0.6040(2) 0.0208(7) Uani 1 1 d . . . H12A H 0.1061 0.3180 0.5670 0.025 Uiso 1 1 calc R . . C2 C 0.7126(5) 0.5657(5) 0.0598(2) 0.0246(8) Uani 1 1 d . . . C1 C 0.7823(5) 0.5694(5) -0.0131(2) 0.0244(8) Uani 1 1 d . . . C8 C 0.8603(5) 0.5747(5) -0.0969(2) 0.0227(7) Uani 1 1 d . . . C9 C 0.9277(5) 0.5780(5) -0.1706(2) 0.0220(7) Uani 1 1 d . . . P1 P 0.26427(13) 0.06238(12) 0.40473(6) 0.0234(2) Uani 1 1 d . . . F2 F 0.2895(4) -0.0632(3) 0.46447(17) 0.0437(6) Uani 1 1 d . . . F1 F 0.0475(4) 0.0056(3) 0.3982(2) 0.0523(7) Uani 1 1 d . . . O1 O 0.3332(4) 0.2412(3) 0.45816(19) 0.0345(6) Uani 1 1 d . . . O2 O 0.3250(5) 0.0096(4) 0.31228(19) 0.0478(8) Uani 1 1 d . . . N1S N 0.7256(8) 1.0212(6) 0.0661(3) 0.0643(13) Uani 1 1 d . . . C1S C 0.7531(7) 1.0448(6) -0.0049(3) 0.0445(11) Uani 1 1 d . . . C2S C 0.7893(9) 1.0785(8) -0.0976(4) 0.0672(17) Uani 1 1 d . . . H2SC H 0.6760 1.0264 -0.1373 0.101 Uiso 1 1 calc R . . H2SB H 0.8844 1.0297 -0.1226 0.101 Uiso 1 1 calc R . . H2SA H 0.8314 1.2014 -0.0937 0.101 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 0.02592(17) 0.03539(18) 0.01327(15) 0.00885(11) 0.01226(10) 0.01093(12) N1 0.0213(14) 0.0289(16) 0.0124(13) 0.0077(12) 0.0081(11) 0.0091(12) C6 0.035(2) 0.0258(19) 0.0196(17) 0.0067(14) 0.0130(15) 0.0160(16) C7 0.034(2) 0.0265(19) 0.0250(19) 0.0146(15) 0.0133(16) 0.0116(16) C3 0.0181(16) 0.032(2) 0.0118(15) 0.0069(14) 0.0061(13) 0.0079(15) C4 0.0227(17) 0.0249(18) 0.0163(16) 0.0029(14) 0.0051(13) 0.0098(15) C5 0.0202(17) 0.0247(18) 0.0178(16) 0.0086(14) 0.0061(13) 0.0058(14) N2 0.0175(14) 0.0300(16) 0.0135(13) 0.0075(12) 0.0078(11) 0.0083(12) C13 0.0292(19) 0.0280(19) 0.0188(17) 0.0095(15) 0.0093(14) 0.0113(16) C14 0.035(2) 0.0242(19) 0.0201(17) 0.0078(14) 0.0115(15) 0.0145(16) C10 0.0169(16) 0.0320(19) 0.0111(15) 0.0075(14) 0.0066(13) 0.0077(14) C11 0.0232(17) 0.0245(18) 0.0154(16) 0.0058(14) 0.0063(13) 0.0032(14) C12 0.0215(17) 0.0252(18) 0.0152(16) 0.0050(14) 0.0060(13) 0.0062(14) C2 0.0238(18) 0.033(2) 0.0185(17) 0.0099(15) 0.0046(14) 0.0083(16) C1 0.0230(18) 0.033(2) 0.0166(17) 0.0071(15) 0.0074(14) 0.0070(16) C8 0.0230(17) 0.030(2) 0.0149(17) 0.0062(14) 0.0050(14) 0.0072(15) C9 0.0200(17) 0.0289(19) 0.0176(17) 0.0073(14) 0.0067(14) 0.0067(15) P1 0.0300(5) 0.0180(5) 0.0222(5) 0.0052(4) 0.0073(4) 0.0071(4) F2 0.0572(16) 0.0431(15) 0.0404(14) 0.0261(12) 0.0096(12) 0.0181(13) F1 0.0322(13) 0.0363(14) 0.086(2) 0.0141(14) -0.0027(13) 0.0062(11) O1 0.0401(16) 0.0261(15) 0.0329(15) 0.0011(12) 0.0102(12) 0.0073(13) O2 0.091(3) 0.0354(17) 0.0227(14) 0.0062(12) 0.0209(15) 0.0285(17) N1S 0.097(4) 0.049(3) 0.042(3) 0.020(2) 0.012(2) 0.007(2) C1S 0.060(3) 0.029(2) 0.036(3) 0.0042(19) -0.002(2) 0.003(2) C2S 0.077(4) 0.069(4) 0.039(3) 0.020(3) 0.000(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.185(3) . y Ag1 N2 2.186(3) . y Ag1 Ag1 3.1927(10) 2_666 y N1 C6 1.339(5) . ? N1 C5 1.345(5) . ? C6 C7 1.377(5) . ? C7 C3 1.394(5) . ? C3 C4 1.392(5) . ? C3 C2 1.436(5) . ? C4 C5 1.382(5) . ? N2 C13 1.338(5) . ? N2 C12 1.343(4) . ? C13 C14 1.383(5) . ? C14 C10 1.398(5) . ? C10 C11 1.392(5) . ? C10 C9 1.425(4) 1_456 ? C11 C12 1.379(5) . ? C2 C1 1.197(5) . ? C1 C8 1.370(5) . ? C8 C9 1.199(5) . ? C9 C10 1.425(4) 1_654 ? P1 O2 1.459(3) . ? P1 O1 1.460(3) . ? P1 F1 1.544(3) . ? P1 F2 1.545(2) . ? N1S C1S 1.110(6) . ? C1S C2S 1.458(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 169.88(10) . . y N1 Ag1 Ag1 97.04(8) . 2_666 y N2 Ag1 Ag1 92.96(8) . 2_666 y C6 N1 C5 118.2(3) . . ? C6 N1 Ag1 120.1(2) . . ? C5 N1 Ag1 121.7(2) . . ? N1 C6 C7 122.8(3) . . ? C6 C7 C3 119.0(3) . . ? C4 C3 C7 118.5(3) . . ? C4 C3 C2 121.2(3) . . ? C7 C3 C2 120.4(3) . . ? C5 C4 C3 118.7(3) . . ? N1 C5 C4 122.8(3) . . ? C13 N2 C12 118.2(3) . . ? C13 N2 Ag1 122.4(2) . . ? C12 N2 Ag1 119.1(2) . . ? N2 C13 C14 123.2(3) . . ? C13 C14 C10 118.4(3) . . ? C11 C10 C14 118.2(3) . . ? C11 C10 C9 120.4(3) . 1_456 ? C14 C10 C9 121.4(3) . 1_456 ? C12 C11 C10 119.4(3) . . ? N2 C12 C11 122.4(3) . . ? C1 C2 C3 179.6(4) . . ? C2 C1 C8 179.2(4) . . ? C9 C8 C1 179.5(4) . . ? C8 C9 C10 177.8(4) . 1_654 ? O2 P1 O1 122.10(18) . . ? O2 P1 F1 108.0(2) . . ? O1 P1 F1 108.03(17) . . ? O2 P1 F2 108.10(17) . . ? O1 P1 F2 110.07(16) . . ? F1 P1 F2 97.75(16) . . ? N1S C1S C2S 179.2(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ag1 N1 C6 70.3(7) . . . . ? Ag1 Ag1 N1 C6 -118.6(3) 2_666 . . . ? N2 Ag1 N1 C5 -110.8(6) . . . . ? Ag1 Ag1 N1 C5 60.3(3) 2_666 . . . ? C5 N1 C6 C7 -0.8(5) . . . . ? Ag1 N1 C6 C7 178.2(3) . . . . ? N1 C6 C7 C3 0.2(6) . . . . ? C6 C7 C3 C4 0.2(5) . . . . ? C6 C7 C3 C2 -179.8(3) . . . . ? C7 C3 C4 C5 0.0(5) . . . . ? C2 C3 C4 C5 -180.0(3) . . . . ? C6 N1 C5 C4 1.0(5) . . . . ? Ag1 N1 C5 C4 -177.9(2) . . . . ? C3 C4 C5 N1 -0.6(5) . . . . ? N1 Ag1 N2 C13 -78.6(7) . . . . ? Ag1 Ag1 N2 C13 110.3(3) 2_666 . . . ? N1 Ag1 N2 C12 106.6(6) . . . . ? Ag1 Ag1 N2 C12 -64.6(2) 2_666 . . . ? C12 N2 C13 C14 1.5(5) . . . . ? Ag1 N2 C13 C14 -173.4(3) . . . . ? N2 C13 C14 C10 -0.1(6) . . . . ? C13 C14 C10 C11 -1.6(5) . . . . ? C13 C14 C10 C9 177.0(3) . . . 1_456 ? C14 C10 C11 C12 1.9(5) . . . . ? C9 C10 C11 C12 -176.7(3) 1_456 . . . ? C13 N2 C12 C11 -1.2(5) . . . . ? Ag1 N2 C12 C11 173.8(3) . . . . ? C10 C11 C12 N2 -0.5(5) . . . . ? C4 C3 C2 C1 130(80) . . . . ? C7 C3 C2 C1 -50(80) . . . . ? C3 C2 C1 C8 -3(100) . . . . ? C2 C1 C8 C9 -96(61) . . . . ? C1 C8 C9 C10 -58(54) . . . 1_654 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.16 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.91 _refine_diff_density_min -1.11 _refine_diff_density_rms 0.09 #===END data_agynac _audit_creation_method SHELXL-97 _chemical_name_systematic ; [1,4-Bis(4'-pyridyl)butadiynesilver(I)] acetate tris(hydrate) methanol solvate ; _chemical_name_common '[agdbp]Ac' _chemical_melting_point unknown _chemical_formula_moiety 'C14 H8 N2 Ag+, C2 H3 O2 -, C1.17 H4.68 O1.17, H3.5 O1.75' _chemical_formula_sum 'C17.17 H19.18 Ag N2 O4.92' _chemical_formula_weight 440.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8638(12) _cell_length_b 14.1102(12) _cell_length_c 15.8947(13) _cell_angle_alpha 82.284(2) _cell_angle_beta 89.338(2) _cell_angle_gamma 72.359(2) _cell_volume 2934.9(4) _cell_formula_units_Z 6 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5901 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.53 _exptl_crystal_description 'irregular plate' _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.773 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 20 _diffrn_standards_decay_% none _diffrn_reflns_number 29777 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.80 _reflns_number_total 13436 _reflns_number_gt 11131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT version 6.01 (Bruker, 1999)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL97; PLATON (Spek, 2000)' _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^)+(0.076P)^2^+9.512P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens ; aromatic placed geometrically, Me-groups of MeCOO from delta-F synthesis, water have distance restraints, others not found ; _refine_ls_hydrogen_treatment 'riding model for aromatic, rigid rotator for Me-groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11420 _refine_ls_number_parameters 723 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag -0.01383(2) 0.42039(2) 0.918413(19) 0.02962(9) Uani 1 1 d . . . Ag2 Ag -0.04408(2) 0.30895(2) 0.76746(2) 0.03075(9) Uani 1 1 d . . . Ag3 Ag 0.07367(2) 0.01719(2) 0.56469(2) 0.03510(10) Uani 1 1 d . . . N101 N 0.1166(2) 0.2844(2) 0.9301(2) 0.0276(7) Uani 1 1 d . . . N102 N 0.8521(2) -0.4522(2) 0.9348(2) 0.0263(7) Uani 1 1 d . . . N201 N 0.0860(2) 0.1799(2) 0.7454(2) 0.0258(6) Uani 1 1 d . . . N202 N 0.8225(2) -0.5569(2) 0.7498(2) 0.0261(6) Uani 1 1 d . . . N301 N -0.7959(2) 0.8801(3) 0.5761(2) 0.0336(8) Uani 1 1 d . . . N302 N -0.0533(2) 0.1467(2) 0.5896(2) 0.0278(7) Uani 1 1 d . . . O1 O 0.0597(3) 0.5287(2) 0.8166(2) 0.0436(7) Uani 1 1 d . . . O2 O 0.0660(2) 0.4364(2) 0.71276(19) 0.0372(7) Uani 1 1 d . . . O3 O -0.1209(2) 0.2018(2) 0.8708(2) 0.0407(7) Uani 1 1 d . . . O4 O -0.1279(2) 0.3012(2) 0.9691(2) 0.0372(7) Uani 1 1 d . . . O5 O 0.1580(3) 0.1165(3) 0.4630(2) 0.0632(10) Uani 1 1 d . . . O6 O 0.0456(3) 0.1003(3) 0.3741(2) 0.0529(9) Uani 1 1 d . . . C1A C 0.0649(3) 0.5156(3) 0.7399(3) 0.0318(8) Uani 1 1 d . . . C2A C 0.0663(6) 0.6042(4) 0.6758(4) 0.0656(17) Uani 1 1 d . . . H2AC H 0.1323 0.5901 0.6491 0.098 Uiso 1 1 calc R . . H2AB H 0.0546 0.6638 0.7044 0.098 Uiso 1 1 calc R . . H2AA H 0.0129 0.6162 0.6322 0.098 Uiso 1 1 calc R . . C3A C -0.1314(3) 0.2215(3) 0.9457(3) 0.0329(9) Uani 1 1 d . . . C4A C -0.1521(6) 0.1438(4) 1.0116(3) 0.0700(19) Uani 1 1 d . . . H4AC H -0.2153 0.1318 0.9963 0.105 Uiso 1 1 calc R . . H4AB H -0.1584 0.1677 1.0671 0.105 Uiso 1 1 calc R . . H4AA H -0.0961 0.0811 1.0143 0.105 Uiso 1 1 calc R . . C5A C 0.1211(4) 0.1228(3) 0.3905(3) 0.0421(10) Uani 1 1 d . . . C6A C 0.1781(6) 0.1603(6) 0.3170(4) 0.073(2) Uani 1 1 d . . . H6AC H 0.2429 0.1634 0.3385 0.110 Uiso 1 1 calc R . . H6AB H 0.1375 0.2273 0.2911 0.110 Uiso 1 1 calc R . . H6AA H 0.1905 0.1141 0.2744 0.110 Uiso 1 1 calc R . . C101 C 0.4292(3) -0.0575(3) 0.9417(3) 0.0320(9) Uani 1 1 d . . . C102 C 0.3602(3) 0.0187(3) 0.9406(3) 0.0320(9) Uani 1 1 d . . . C103 C 0.2781(3) 0.1091(3) 0.9385(2) 0.0265(8) Uani 1 1 d . . . C104 C 0.1973(3) 0.1144(3) 0.9922(3) 0.0281(8) Uani 1 1 d . . . H104 H 0.1961 0.0585 1.0324 0.034 Uiso 1 1 calc R . . C105 C 0.1188(3) 0.2033(3) 0.9855(2) 0.0273(8) Uani 1 1 d . . . H105 H 0.0635 0.2071 1.0221 0.033 Uiso 1 1 calc R . . C106 C 0.1957(3) 0.2791(3) 0.8802(2) 0.0291(8) Uani 1 1 d . . . H106 H 0.1958 0.3368 0.8418 0.035 Uiso 1 1 calc R . . C107 C 0.2771(3) 0.1937(3) 0.8818(3) 0.0302(8) Uani 1 1 d . . . H107 H 0.3317 0.1926 0.8448 0.036 Uiso 1 1 calc R . . C108 C 0.5104(3) -0.1416(3) 0.9422(3) 0.0321(9) Uani 1 1 d . . . C109 C 0.5835(3) -0.2136(3) 0.9419(3) 0.0322(9) Uani 1 1 d . . . C110 C 0.6738(3) -0.2949(3) 0.9397(3) 0.0282(8) Uani 1 1 d . . . C111 C 0.7504(3) -0.2856(3) 0.8851(3) 0.0294(8) Uani 1 1 d . . . H111 H 0.7425 -0.2248 0.8480 0.035 Uiso 1 1 calc R . . C112 C 0.8378(3) -0.3648(3) 0.8847(3) 0.0275(8) Uani 1 1 d . . . H112 H 0.8898 -0.3570 0.8475 0.033 Uiso 1 1 calc R . . C113 C 0.7783(3) -0.4618(3) 0.9872(3) 0.0319(8) Uani 1 1 d . . . H113 H 0.7880 -0.5236 1.0232 0.038 Uiso 1 1 calc R . . C114 C 0.6886(3) -0.3857(3) 0.9913(3) 0.0324(9) Uani 1 1 d . . . H114 H 0.6377 -0.3955 1.0290 0.039 Uiso 1 1 calc R . . C201 C 0.4196(3) -0.1372(3) 0.7280(3) 0.0337(9) Uani 1 1 d . . . C202 C 0.3455(3) -0.0659(3) 0.7284(3) 0.0320(8) Uani 1 1 d . . . C203 C 0.2565(3) 0.0173(3) 0.7314(2) 0.0277(8) Uani 1 1 d . . . C204 C 0.1760(3) 0.0059(3) 0.7798(3) 0.0330(9) Uani 1 1 d . . . H204 H 0.1778 -0.0582 0.8085 0.040 Uiso 1 1 calc R . . C205 C 0.0929(3) 0.0888(3) 0.7858(3) 0.0283(8) Uani 1 1 d . . . H205 H 0.0386 0.0805 0.8200 0.034 Uiso 1 1 calc R . . C206 C 0.1623(3) 0.1896(3) 0.6966(3) 0.0327(9) Uani 1 1 d . . . H206 H 0.1569 0.2538 0.6664 0.039 Uiso 1 1 calc R . . C207 C 0.2484(3) 0.1119(3) 0.6877(3) 0.0346(9) Uani 1 1 d . . . H207 H 0.3010 0.1225 0.6524 0.042 Uiso 1 1 calc R . . C208 C 0.5017(3) -0.2207(3) 0.7290(3) 0.0335(9) Uani 1 1 d . . . C209 C 0.5725(3) -0.2957(3) 0.7308(3) 0.0328(9) Uani 1 1 d . . . C210 C 0.6562(3) -0.3850(3) 0.7352(2) 0.0268(8) Uani 1 1 d . . . C211 C 0.7356(3) -0.3921(3) 0.6801(3) 0.0304(8) Uani 1 1 d . . . H211 H 0.7341 -0.3384 0.6366 0.036 Uiso 1 1 calc R . . C212 C 0.8172(3) -0.4789(3) 0.6897(2) 0.0288(8) Uani 1 1 d . . . H212 H 0.8718 -0.4833 0.6522 0.035 Uiso 1 1 calc R . . C213 C 0.7450(3) -0.5512(3) 0.8010(3) 0.0295(8) Uani 1 1 d . . . H213 H 0.7478 -0.6068 0.8429 0.035 Uiso 1 1 calc R . . C214 C 0.6603(3) -0.4671(3) 0.7957(3) 0.0308(8) Uani 1 1 d . . . H214 H 0.6060 -0.4656 0.8330 0.037 Uiso 1 1 calc R . . C301 C -0.4739(3) 0.5444(4) 0.5942(3) 0.0481(12) Uani 1 1 d . . . C302 C -0.5464(3) 0.6176(4) 0.5910(4) 0.0489(13) Uani 1 1 d . . . C303 C -0.6314(3) 0.7067(3) 0.5862(3) 0.0415(11) Uani 1 1 d . . . C304 C -0.7161(4) 0.7098(4) 0.6344(4) 0.0575(15) Uani 1 1 d . . . H304 H -0.7193 0.6523 0.6717 0.069 Uiso 1 1 calc R . . C305 C -0.7954(3) 0.7975(3) 0.6272(4) 0.0525(14) Uani 1 1 d . . . H305 H -0.8529 0.7990 0.6607 0.063 Uiso 1 1 calc R . . C306 C -0.7143(3) 0.8766(4) 0.5307(3) 0.0456(11) Uani 1 1 d . . . H306 H -0.7132 0.9351 0.4938 0.055 Uiso 1 1 calc R . . C307 C -0.6313(4) 0.7927(4) 0.5343(3) 0.0522(13) Uani 1 1 d . . . H307 H -0.5742 0.7941 0.5010 0.063 Uiso 1 1 calc R . . C308 C -0.3900(3) 0.4619(4) 0.5975(3) 0.0433(11) Uani 1 1 d . . . C309 C -0.3144(3) 0.3921(3) 0.5994(3) 0.0392(10) Uani 1 1 d . . . C310 C -0.2245(3) 0.3102(3) 0.5992(3) 0.0336(9) Uani 1 1 d . . . C311 C -0.1419(4) 0.3213(3) 0.5526(3) 0.0403(10) Uani 1 1 d . . . H311 H -0.1431 0.3850 0.5235 0.048 Uiso 1 1 calc R . . C312 C -0.0588(3) 0.2389(3) 0.5492(3) 0.0383(10) Uani 1 1 d . . . H312 H -0.0028 0.2470 0.5172 0.046 Uiso 1 1 calc R . . C313 C -0.1295(3) 0.1385(3) 0.6364(3) 0.0371(9) Uani 1 1 d . . . H313 H -0.1250 0.0747 0.6673 0.045 Uiso 1 1 calc R . . C314 C -0.2159(3) 0.2171(3) 0.6433(3) 0.0416(10) Uani 1 1 d . . . H314 H -0.2690 0.2070 0.6782 0.050 Uiso 1 1 calc R . . O1W O 0.7718(4) 0.7341(4) 0.5027(3) 0.0760(13) Uani 1 1 d D . . H1WA H 0.813(5) 0.759(6) 0.524(4) 0.114 Uiso 1 1 d D . . H1WB H 0.755(6) 0.770(5) 0.455(3) 0.114 Uiso 1 1 d D . . O2W O -0.0038(3) 0.1068(3) 0.2082(3) 0.0631(10) Uani 1 1 d D . . H2WA H 0.013(6) 0.108(5) 0.2593(16) 0.095 Uiso 1 1 d D . . H2WB H -0.020(6) 0.1680(17) 0.186(4) 0.095 Uiso 1 1 d D . . O3W O -0.0900(4) 0.3020(3) 0.1365(3) 0.0653(11) Uani 1 1 d D . . H3WA H -0.076(6) 0.353(3) 0.147(4) 0.098 Uiso 1 1 d D . . H3WB H -0.105(6) 0.313(5) 0.0838(13) 0.098 Uiso 1 1 d D . . O4W O -0.1696(3) 0.0358(3) 0.8355(2) 0.0501(8) Uani 1 1 d D . . H4WA H -0.1087(15) 0.002(4) 0.830(3) 0.075 Uiso 1 1 d D . . H4WB H -0.200(4) 0.038(5) 0.789(2) 0.075 Uiso 1 1 d D . . O5W O 0.9195(5) 0.5690(4) 0.4584(3) 0.0900(17) Uani 1 1 d D . . H5WA H 0.949(6) 0.579(6) 0.413(3) 0.135 Uiso 1 1 d D . . H5WB H 0.869(5) 0.621(4) 0.459(5) 0.135 Uiso 1 1 d D . . O5M O 0.3446(7) 0.9329(7) 0.2520(6) 0.109(3) Uiso 0.67 1 d P . . C5M C 0.4063(12) 0.9716(12) 0.1866(11) 0.046(3) Uiso 0.33 1 d P A 1 C5M' C 0.417(2) 0.971(2) 0.2275(18) 0.088(7) Uiso 0.33 1 d P A 2 O4M O 0.4282(16) 0.7112(16) 0.1532(13) 0.181(7) Uiso 0.50 1 d P . . C4M C 0.5062(17) 0.6188(18) 0.1762(14) 0.055(5) Uiso 0.25 1 d P B 1 C4M' C 0.431(3) 0.813(3) 0.173(3) 0.117(12) Uiso 0.25 1 d P B 2 O2M O 0.560(3) 0.924(3) 0.501(3) 0.38(2) Uiso 0.50 1 d P . . C2M' C 0.583(2) 0.873(2) 0.479(2) 0.077(8) Uiso 0.25 1 d P C 1 C2M C 0.425(2) 0.987(2) 0.393(2) 0.086(8) Uiso 0.25 1 d P D 2 C3M C 0.6388(14) 0.6292(15) 0.3883(13) 0.223(9) Uani 1 1 d . . . O3M O 0.5242(11) 0.7488(11) 0.3409(9) 0.120(4) Uiso 0.50 1 d P E 1 O3M' O 0.7013(14) 0.5941(14) 0.3271(12) 0.150(6) Uiso 0.50 1 d P F 2 O1M O 0.6144(11) 0.4441(11) 0.1606(9) 0.048(3) Uiso 0.25 1 d P G 1 C1M C 0.6164(14) 0.3628(13) 0.0928(15) 0.034(4) Uiso 0.25 1 d P G 1 O1M' C 0.6373(11) 0.4734(11) 0.1924(9) 0.023(3) Uiso 0.25 1 d P H 2 O6M O 0.5972(10) 0.3799(10) 0.0490(9) 0.062(3) Uiso 0.33 1 d P I 3 C6M C 0.6372(18) 0.3705(17) 0.1271(16) 0.074(6) Uiso 0.33 1 d P I 3 O6W O 0.5309(9) 0.5356(9) 0.1226(7) 0.097(3) Uiso 0.50 1 d P J 4 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 0.02039(15) 0.02000(15) 0.04002(18) -0.00497(12) 0.00071(12) 0.00675(11) Ag2 0.02128(15) 0.02358(15) 0.03881(18) -0.00769(12) -0.00108(12) 0.00741(11) Ag3 0.02494(16) 0.02633(16) 0.04453(19) -0.00878(13) -0.00069(13) 0.00803(12) N101 0.0197(15) 0.0169(14) 0.0409(18) -0.0084(13) -0.0022(13) 0.0041(12) N102 0.0227(15) 0.0162(14) 0.0354(17) -0.0074(13) 0.0007(13) 0.0023(12) N201 0.0210(15) 0.0191(14) 0.0320(16) -0.0052(12) 0.0018(12) 0.0026(12) N202 0.0196(15) 0.0217(15) 0.0320(17) -0.0059(13) -0.0022(12) 0.0020(12) N301 0.0215(16) 0.0272(17) 0.047(2) -0.0129(15) -0.0057(14) 0.0038(13) N302 0.0239(16) 0.0278(17) 0.0238(15) -0.0028(13) -0.0020(12) 0.0034(13) O1 0.054(2) 0.0332(16) 0.0409(18) -0.0045(13) 0.0090(15) -0.0102(14) O2 0.0382(16) 0.0263(14) 0.0436(17) -0.0003(12) -0.0024(13) -0.0064(12) O3 0.0477(18) 0.0324(15) 0.0396(17) -0.0058(13) 0.0143(14) -0.0087(13) O4 0.0340(16) 0.0290(15) 0.0465(17) -0.0023(13) -0.0008(13) -0.0075(12) O5 0.077(3) 0.060(2) 0.047(2) -0.0035(18) 0.0105(19) -0.014(2) O6 0.053(2) 0.0394(18) 0.063(2) -0.0034(16) 0.0201(17) -0.0116(16) C1A 0.0260(19) 0.027(2) 0.037(2) 0.0016(17) 0.0043(16) -0.0040(15) C2A 0.109(5) 0.047(3) 0.051(3) -0.001(2) 0.013(3) -0.041(3) C3A 0.028(2) 0.028(2) 0.041(2) -0.0019(17) 0.0026(17) -0.0064(16) C4A 0.134(6) 0.053(3) 0.040(3) -0.003(2) 0.009(3) -0.055(4) C5A 0.047(3) 0.035(2) 0.041(3) -0.0063(19) 0.009(2) -0.007(2) C6A 0.094(5) 0.105(5) 0.046(3) -0.014(3) 0.018(3) -0.065(4) C101 0.0235(19) 0.027(2) 0.040(2) -0.0099(17) -0.0041(16) 0.0030(16) C102 0.0239(19) 0.027(2) 0.041(2) -0.0117(17) -0.0039(16) 0.0020(16) C103 0.0183(17) 0.0224(18) 0.034(2) -0.0104(15) -0.0069(14) 0.0031(14) C104 0.0269(19) 0.0189(17) 0.035(2) -0.0043(15) -0.0027(15) -0.0011(14) C105 0.0205(17) 0.0251(18) 0.033(2) -0.0057(15) 0.0011(15) -0.0019(14) C106 0.0245(19) 0.0265(19) 0.0294(19) -0.0006(15) 0.0003(15) 0.0013(15) C107 0.0206(18) 0.032(2) 0.034(2) -0.0084(16) 0.0022(15) -0.0008(15) C108 0.0244(19) 0.028(2) 0.039(2) -0.0107(17) -0.0021(16) 0.0020(16) C109 0.0245(19) 0.0259(19) 0.040(2) -0.0111(17) -0.0044(16) 0.0040(16) C110 0.0232(18) 0.0217(18) 0.035(2) -0.0124(15) -0.0051(15) 0.0039(14) C111 0.0277(19) 0.0200(17) 0.034(2) -0.0039(15) -0.0030(16) 0.0022(15) C112 0.0243(18) 0.0196(17) 0.035(2) -0.0055(15) -0.0024(15) -0.0002(14) C113 0.028(2) 0.0202(18) 0.042(2) -0.0046(16) 0.0034(17) 0.0007(15) C114 0.0232(19) 0.0269(19) 0.042(2) -0.0079(17) 0.0057(16) 0.0006(15) C201 0.029(2) 0.030(2) 0.035(2) -0.0113(17) -0.0058(16) 0.0036(17) C202 0.0253(19) 0.029(2) 0.036(2) -0.0110(16) -0.0033(16) 0.0038(16) C203 0.0218(18) 0.0248(18) 0.0309(19) -0.0105(15) -0.0023(15) 0.0043(15) C204 0.032(2) 0.0199(18) 0.040(2) -0.0021(16) 0.0014(17) 0.0004(15) C205 0.0231(18) 0.0240(18) 0.035(2) -0.0054(15) 0.0058(15) -0.0029(15) C206 0.028(2) 0.0259(19) 0.035(2) 0.0008(16) 0.0051(16) 0.0027(16) C207 0.029(2) 0.032(2) 0.035(2) -0.0028(17) 0.0071(16) 0.0019(16) C208 0.026(2) 0.030(2) 0.039(2) -0.0127(17) -0.0062(16) 0.0032(16) C209 0.0253(19) 0.030(2) 0.037(2) -0.0132(17) -0.0066(16) 0.0041(16) C210 0.0213(18) 0.0226(18) 0.0312(19) -0.0111(15) -0.0063(14) 0.0047(14) C211 0.0265(19) 0.0247(18) 0.034(2) -0.0024(15) -0.0050(16) 0.0006(15) C212 0.0212(18) 0.0279(19) 0.032(2) -0.0060(16) 0.0005(15) 0.0007(15) C213 0.0239(18) 0.0276(19) 0.033(2) -0.0048(16) -0.0009(15) -0.0013(15) C214 0.0225(18) 0.033(2) 0.033(2) -0.0111(16) 0.0023(15) -0.0003(16) C301 0.031(2) 0.042(3) 0.065(3) -0.030(2) -0.016(2) 0.008(2) C302 0.030(2) 0.042(3) 0.068(3) -0.031(2) -0.020(2) 0.010(2) C303 0.024(2) 0.035(2) 0.060(3) -0.025(2) -0.0168(19) 0.0087(17) C304 0.030(2) 0.025(2) 0.111(5) -0.009(3) -0.006(3) 0.0009(18) C305 0.025(2) 0.028(2) 0.100(4) -0.008(2) 0.005(2) -0.0021(18) C306 0.032(2) 0.046(3) 0.045(3) -0.007(2) 0.0033(19) 0.008(2) C307 0.035(2) 0.057(3) 0.047(3) -0.014(2) 0.004(2) 0.014(2) C308 0.030(2) 0.039(2) 0.056(3) -0.025(2) -0.013(2) 0.0067(19) C309 0.030(2) 0.038(2) 0.042(2) -0.0190(19) -0.0100(18) 0.0075(18) C310 0.028(2) 0.031(2) 0.035(2) -0.0156(17) -0.0084(16) 0.0068(16) C311 0.044(2) 0.025(2) 0.039(2) -0.0019(17) 0.0035(19) 0.0071(18) C312 0.036(2) 0.028(2) 0.042(2) -0.0040(18) 0.0081(18) 0.0041(17) C313 0.032(2) 0.027(2) 0.046(2) -0.0032(18) 0.0048(18) -0.0001(17) C314 0.030(2) 0.035(2) 0.053(3) -0.011(2) 0.0087(19) 0.0008(18) O1W 0.094(4) 0.086(3) 0.052(2) -0.007(2) 0.015(2) -0.035(3) O2W 0.066(3) 0.0381(19) 0.082(3) -0.0064(19) -0.009(2) -0.0108(18) O3W 0.103(3) 0.0332(18) 0.057(2) -0.0063(16) -0.021(2) -0.016(2) O4W 0.055(2) 0.052(2) 0.049(2) -0.0121(17) 0.0110(16) -0.0219(18) O5W 0.110(4) 0.076(3) 0.052(2) -0.018(2) -0.016(3) 0.023(3) C3M 0.188(16) 0.27(2) 0.27(2) -0.136(18) -0.004(15) -0.106(16) _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 N101 2.190(3) . y Ag1 N102 2.201(3) 1_465 y Ag1 O1 2.497(3) . y Ag1 Ag2 3.1371(5) . y Ag2 O3 2.527(3) . y Ag3 N302 2.196(3) . y Ag3 N301 2.200(3) 1_645 y Ag3 O5 2.507(4) . y Ag3 Ag3 3.0988(7) 2_556 y N101 C106 1.335(5) . ? N101 C105 1.340(5) . ? N102 C112 1.335(5) . ? N102 C113 1.340(5) . ? N102 Ag1 2.201(3) 1_645 ? N201 C205 1.333(5) . ? N201 C206 1.334(5) . ? N202 C213 1.330(5) . ? N202 C212 1.342(5) . ? N202 Ag2 2.198(3) 1_645 ? N301 C306 1.326(6) . ? N301 C305 1.327(6) . ? N301 Ag3 2.200(3) 1_465 ? N302 C313 1.309(5) . ? N302 C312 1.352(5) . ? O1 C1A 1.256(5) . ? O2 C1A 1.246(5) . ? O3 C3A 1.256(5) . ? O4 C3A 1.246(5) . ? O5 C5A 1.248(6) . ? O6 C5A 1.223(6) . ? C1A C2A 1.508(6) . ? C2A H2AC 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AA 0.9800 . ? C3A C4A 1.502(6) . ? C4A H4AC 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AA 0.9800 . ? C5A C6A 1.527(7) . ? C6A H6AC 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AA 0.9800 . ? C101 C102 1.201(6) . ? C101 C108 1.365(5) . ? C102 C103 1.426(5) . ? C103 C104 1.391(6) . ? C103 C107 1.393(6) . ? C104 C105 1.381(5) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 C107 1.376(5) . ? C106 H106 0.9500 . ? C107 H107 0.9500 . ? C108 C109 1.199(6) . ? C109 C110 1.423(5) . ? C110 C114 1.385(6) . ? C110 C111 1.390(6) . ? C111 C112 1.378(5) . ? C111 H111 0.9500 . ? C112 H112 0.9500 . ? C113 C114 1.382(5) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C201 C202 1.201(6) . ? C201 C208 1.366(6) . ? C202 C203 1.428(5) . ? C203 C204 1.384(6) . ? C203 C207 1.394(6) . ? C204 C205 1.384(5) . ? C204 H204 0.9500 . ? C205 H205 0.9500 . ? C206 C207 1.375(5) . ? C206 H206 0.9500 . ? C207 H207 0.9500 . ? C208 C209 1.203(6) . ? C209 C210 1.425(5) . ? C210 C211 1.387(6) . ? C210 C214 1.390(6) . ? C211 C212 1.384(5) . ? C211 H211 0.9500 . ? C212 H212 0.9500 . ? C213 C214 1.387(5) . ? C213 H213 0.9500 . ? C214 H214 0.9500 . ? C301 C302 1.198(6) . ? C301 C308 1.369(6) . ? C302 C303 1.434(6) . ? C303 C307 1.372(8) . ? C303 C304 1.388(8) . ? C304 C305 1.376(6) . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? C306 C307 1.374(6) . ? C306 H306 0.9500 . ? C307 H307 0.9500 . ? C308 C309 1.200(6) . ? C309 C310 1.420(5) . ? C310 C314 1.375(6) . ? C310 C311 1.394(6) . ? C311 C312 1.373(6) . ? C311 H311 0.9500 . ? C312 H312 0.9500 . ? C313 C314 1.379(6) . ? C313 H313 0.9500 . ? C314 H314 0.9500 . ? O1W H1WA 0.856(10) . ? O1W H1WB 0.852(10) . ? O2W H2WA 0.853(10) . ? O2W H2WB 0.850(10) . ? O3W H3WA 0.847(10) . ? O3W H3WB 0.849(10) . ? O4W H4WA 0.844(10) . ? O4W H4WB 0.846(10) . ? O5W H5WA 0.847(10) . ? O5W H5WB 0.846(10) . ? O5M C5M' 1.31(3) . ? O5M C5M 1.491(18) . ? O4M C4M 1.42(3) . ? O4M C4M' 1.52(4) . ? O2M C2M' 0.80(5) . ? C3M O3M' 1.34(2) . ? O1M C1M 1.67(2) . ? O6M C6M 1.34(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 N101 Ag1 N102 168.18(12) . 1_465 y N101 Ag1 O1 97.56(12) . . y N102 Ag1 O1 91.80(11) 1_465 . y N101 Ag1 Ag2 75.49(9) . . y N102 Ag1 Ag2 112.12(8) 1_465 . y O1 Ag1 Ag2 88.53(8) . . y N202 Ag2 N201 163.65(12) 1_465 . y N202 Ag2 O3 96.96(11) 1_465 . y N201 Ag2 O3 92.80(11) . . y N202 Ag2 Ag1 78.43(8) 1_465 . y N201 Ag2 Ag1 115.08(8) . . y O3 Ag2 Ag1 88.14(7) . . y N302 Ag3 N301 165.02(13) . 1_645 y N302 Ag3 O5 95.44(13) . . y N301 Ag3 O5 93.99(14) 1_645 . y N302 Ag3 Ag3 85.58(8) . 2_556 y N301 Ag3 Ag3 104.64(9) 1_645 2_556 y O5 Ag3 Ag3 97.82(10) . 2_556 y C106 N101 C105 117.9(3) . . ? C106 N101 Ag1 120.6(3) . . ? C105 N101 Ag1 121.5(3) . . ? C112 N102 C113 118.0(3) . . ? C112 N102 Ag1 119.4(3) . 1_645 ? C113 N102 Ag1 122.2(2) . 1_645 ? C205 N201 C206 117.8(3) . . ? C205 N201 Ag2 119.5(2) . . ? C206 N201 Ag2 122.6(3) . . ? C213 N202 C212 118.4(3) . . ? C213 N202 Ag2 119.5(3) . 1_645 ? C212 N202 Ag2 122.0(3) . 1_645 ? C306 N301 C305 117.2(4) . . ? C306 N301 Ag3 120.8(3) . 1_465 ? C305 N301 Ag3 122.0(3) . 1_465 ? C313 N302 C312 117.4(3) . . ? C313 N302 Ag3 123.2(3) . . ? C312 N302 Ag3 119.1(3) . . ? C1A O1 Ag1 118.8(3) . . ? C3A O3 Ag2 117.7(3) . . ? C5A O5 Ag3 107.9(3) . . ? O2 C1A O1 125.2(4) . . ? O2 C1A C2A 117.9(4) . . ? O1 C1A C2A 116.9(4) . . ? C1A C2A H2AC 109.5 . . ? C1A C2A H2AB 109.5 . . ? H2AC C2A H2AB 109.5 . . ? C1A C2A H2AA 109.5 . . ? H2AC C2A H2AA 109.5 . . ? H2AB C2A H2AA 109.5 . . ? O4 C3A O3 124.9(4) . . ? O4 C3A C4A 117.7(4) . . ? O3 C3A C4A 117.4(4) . . ? C3A C4A H4AC 109.5 . . ? C3A C4A H4AB 109.5 . . ? H4AC C4A H4AB 109.5 . . ? C3A C4A H4AA 109.5 . . ? H4AC C4A H4AA 109.5 . . ? H4AB C4A H4AA 109.5 . . ? O6 C5A O5 125.7(5) . . ? O6 C5A C6A 118.5(5) . . ? O5 C5A C6A 115.8(5) . . ? C5A C6A H6AC 109.5 . . ? C5A C6A H6AB 109.5 . . ? H6AC C6A H6AB 109.5 . . ? C5A C6A H6AA 109.5 . . ? H6AC C6A H6AA 109.5 . . ? H6AB C6A H6AA 109.5 . . ? C102 C101 C108 177.5(5) . . ? C101 C102 C103 179.5(5) . . ? C104 C103 C107 118.7(3) . . ? C104 C103 C102 120.9(4) . . ? C107 C103 C102 120.3(4) . . ? C105 C104 C103 118.1(4) . . ? C105 C104 H104 120.9 . . ? C103 C104 H104 120.9 . . ? N101 C105 C104 123.4(4) . . ? N101 C105 H105 118.3 . . ? C104 C105 H105 118.3 . . ? N101 C106 C107 123.0(4) . . ? N101 C106 H106 118.5 . . ? C107 C106 H106 118.5 . . ? C106 C107 C103 118.8(4) . . ? C106 C107 H107 120.6 . . ? C103 C107 H107 120.6 . . ? C109 C108 C101 178.0(5) . . ? C108 C109 C110 176.4(5) . . ? C114 C110 C111 117.7(3) . . ? C114 C110 C109 121.6(4) . . ? C111 C110 C109 120.7(4) . . ? C112 C111 C110 119.8(4) . . ? C112 C111 H111 120.1 . . ? C110 C111 H111 120.1 . . ? N102 C112 C111 122.4(4) . . ? N102 C112 H112 118.8 . . ? C111 C112 H112 118.8 . . ? N102 C113 C114 122.9(4) . . ? N102 C113 H113 118.6 . . ? C114 C113 H113 118.6 . . ? C113 C114 C110 119.1(4) . . ? C113 C114 H114 120.4 . . ? C110 C114 H114 120.4 . . ? C202 C201 C208 177.7(5) . . ? C201 C202 C203 178.2(5) . . ? C204 C203 C207 118.1(3) . . ? C204 C203 C202 120.3(4) . . ? C207 C203 C202 121.6(4) . . ? C205 C204 C203 119.3(4) . . ? C205 C204 H204 120.3 . . ? C203 C204 H204 120.3 . . ? N201 C205 C204 122.6(4) . . ? N201 C205 H205 118.7 . . ? C204 C205 H205 118.7 . . ? N201 C206 C207 123.8(4) . . ? N201 C206 H206 118.1 . . ? C207 C206 H206 118.1 . . ? C206 C207 C203 118.4(4) . . ? C206 C207 H207 120.8 . . ? C203 C207 H207 120.8 . . ? C209 C208 C201 178.3(5) . . ? C208 C209 C210 178.6(5) . . ? C211 C210 C214 118.4(3) . . ? C211 C210 C209 121.2(4) . . ? C214 C210 C209 120.4(4) . . ? C212 C211 C210 118.7(4) . . ? C212 C211 H211 120.6 . . ? C210 C211 H211 120.6 . . ? N202 C212 C211 122.8(4) . . ? N202 C212 H212 118.6 . . ? C211 C212 H212 118.6 . . ? N202 C213 C214 122.5(4) . . ? N202 C213 H213 118.7 . . ? C214 C213 H213 118.7 . . ? C213 C214 C210 119.0(4) . . ? C213 C214 H214 120.5 . . ? C210 C214 H214 120.5 . . ? C302 C301 C308 179.0(7) . . ? C301 C302 C303 178.4(7) . . ? C307 C303 C304 117.6(4) . . ? C307 C303 C302 121.0(5) . . ? C304 C303 C302 121.4(5) . . ? C305 C304 C303 118.8(5) . . ? C305 C304 H304 120.6 . . ? C303 C304 H304 120.6 . . ? N301 C305 C304 123.6(5) . . ? N301 C305 H305 118.2 . . ? C304 C305 H305 118.2 . . ? N301 C306 C307 123.3(5) . . ? N301 C306 H306 118.3 . . ? C307 C306 H306 118.4 . . ? C303 C307 C306 119.5(5) . . ? C303 C307 H307 120.2 . . ? C306 C307 H307 120.2 . . ? C309 C308 C301 177.5(6) . . ? C308 C309 C310 178.4(5) . . ? C314 C310 C311 117.5(4) . . ? C314 C310 C309 121.8(4) . . ? C311 C310 C309 120.7(4) . . ? C312 C311 C310 119.2(4) . . ? C312 C311 H311 120.4 . . ? C310 C311 H311 120.4 . . ? N302 C312 C311 122.7(4) . . ? N302 C312 H312 118.7 . . ? C311 C312 H312 118.7 . . ? N302 C313 C314 123.8(4) . . ? N302 C313 H313 118.1 . . ? C314 C313 H313 118.1 . . ? C310 C314 C313 119.4(4) . . ? C310 C314 H314 120.3 . . ? C313 C314 H314 120.3 . . ? H1WA O1W H1WB 103(2) . . ? H2WA O2W H2WB 104(2) . . ? H3WA O3W H3WB 105(2) . . ? H4WA O4W H4WB 106(2) . . ? H5WA O5W H5WB 105(3) . . ? C5M' O5M C5M 26.6(12) . . ? C4M O4M C4M' 125(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.373 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.130 #===END data_AGEYPY _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-Bis(4'-pyridylethynyl)benzenesilver(I) hexafluorophosphate acetonitrile solvate ; _chemical_name_common '{[Ag*PyCCPhCCPy]PF6*CH3CN}n' _chemical_melting_point unknown _chemical_formula_moiety 'C20 H12 N2 Ag +, P F6 -, C2 H3 N' _chemical_formula_sum 'C22 H15 Ag F6 N3 P' _chemical_formula_weight 574.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 9.263(2) _cell_length_b 18.543(4) _cell_length_c 30.160(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.93(3) _cell_angle_gamma 90.00 _cell_volume 5177(2) _cell_formula_units_Z 8 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 13505 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.96 _exptl_crystal_description needle/column _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type nonw _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'Stoe IPDS area detector' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 13505 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.036 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.96 _reflns_number_total 5723 _reflns_number_gt 4492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe & Cie, 1996a)' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'X-RED (Stoe & Cie, 1996b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 1999)' _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^)+(0.099P)^2^+11.519P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier methods' _atom_sites_solution_hydrogens 'aromatic geometrically placed, others from delta-F synthesis' _refine_ls_hydrogen_treatment 'riding model for aromatic, rigid rotator for Me-group' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5723 _refine_ls_number_parameters 299 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1711 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.24647(3) 0.25815(2) 0.085638(10) 0.05260(18) Uani 1 1 d . . . N1 N 0.0897(3) 0.26145(18) 0.13667(11) 0.0399(7) Uani 1 1 d . . . N2 N -1.1026(3) 0.24114(17) 0.53307(11) 0.0384(7) Uani 1 1 d . . . C1 C -0.3004(4) 0.2609(2) 0.26731(14) 0.0448(8) Uani 1 1 d . . . C2 C -0.2169(4) 0.2617(2) 0.23832(14) 0.0421(8) Uani 1 1 d . . . C3 C -0.1129(4) 0.2625(2) 0.20359(13) 0.0393(8) Uani 1 1 d . . . C4 C -0.0648(4) 0.1980(2) 0.18566(13) 0.0464(8) Uani 1 1 d . . . H4A H -0.0997 0.1531 0.1961 0.056 Uiso 1 1 calc R . . C5 C 0.0353(4) 0.2003(2) 0.15217(13) 0.0464(8) Uani 1 1 d . . . H5A H 0.0663 0.1561 0.1398 0.056 Uiso 1 1 calc R . . C6 C 0.0436(4) 0.3239(2) 0.15406(13) 0.0449(8) Uani 1 1 d . . . H6A H 0.0811 0.3680 0.1433 0.054 Uiso 1 1 calc R . . C7 C -0.0573(4) 0.3260(2) 0.18727(13) 0.0448(8) Uani 1 1 d . . . H7A H -0.0878 0.3710 0.1987 0.054 Uiso 1 1 calc R . . C8 C -0.4017(4) 0.2589(2) 0.30231(13) 0.0423(8) Uani 1 1 d . . . C9 C -0.4523(5) 0.1933(3) 0.31842(15) 0.0512(9) Uani 1 1 d . . . H9A H -0.4188 0.1495 0.3062 0.061 Uiso 1 1 calc R . . C10 C -0.5509(4) 0.1911(3) 0.35203(15) 0.0512(10) Uani 1 1 d . . . H10A H -0.5835 0.1461 0.3629 0.061 Uiso 1 1 calc R . . C11 C -0.6021(4) 0.2555(2) 0.36983(13) 0.0427(9) Uani 1 1 d . . . C12 C -0.5494(5) 0.3212(3) 0.35435(15) 0.0523(10) Uani 1 1 d . . . H12A H -0.5809 0.3651 0.3672 0.063 Uiso 1 1 calc R . . C13 C -0.4513(5) 0.3231(3) 0.32033(15) 0.0524(10) Uani 1 1 d . . . H13A H -0.4183 0.3680 0.3095 0.063 Uiso 1 1 calc R . . C14 C -0.7065(5) 0.2539(2) 0.40372(15) 0.0454(9) Uani 1 1 d . . . C15 C -0.7969(5) 0.2508(2) 0.43184(15) 0.0447(9) Uani 1 1 d . . . C16 C -0.9009(4) 0.2471(2) 0.46541(13) 0.0389(8) Uani 1 1 d . . . C17 C -0.9567(4) 0.1812(2) 0.47971(13) 0.0442(8) Uani 1 1 d . . . H17A H -0.9269 0.1372 0.4667 0.053 Uiso 1 1 calc R . . C18 C -1.0566(4) 0.1808(2) 0.51331(13) 0.0429(8) Uani 1 1 d . . . H18A H -1.0938 0.1358 0.5227 0.051 Uiso 1 1 calc R . . C19 C -1.0486(4) 0.3041(2) 0.51935(15) 0.0488(9) Uani 1 1 d . . . H19A H -1.0785 0.3471 0.5335 0.059 Uiso 1 1 calc R . . C20 C -0.9508(5) 0.3094(2) 0.48540(15) 0.0502(9) Uani 1 1 d . . . H20A H -0.9185 0.3554 0.4760 0.060 Uiso 1 1 calc R . . P1 P 0.26335(13) -0.00285(6) 0.42063(4) 0.0565(3) Uani 1 1 d . . . F1 F 0.1886(6) 0.0585(3) 0.39142(19) 0.1344(19) Uani 1 1 d . . . F2 F 0.3360(6) 0.0600(3) 0.44804(17) 0.1209(16) Uani 1 1 d . . . F3 F 0.3963(5) -0.0034(2) 0.38864(17) 0.1152(16) Uani 1 1 d . . . F4 F 0.1304(5) -0.0011(2) 0.45272(17) 0.1098(15) Uani 1 1 d . . . F5 F 0.1896(6) -0.0655(3) 0.3929(2) 0.139(2) Uani 1 1 d . . . F6 F 0.3319(6) -0.0641(3) 0.4490(2) 0.152(2) Uani 1 1 d . . . C2S C 0.2453(10) -0.0300(4) 0.0621(3) 0.105(2) Uani 1 1 d U . . H2SA H 0.1461 -0.0469 0.0565 0.158 Uiso 1 1 calc R . . H2SB H 0.2927 -0.0602 0.0850 0.158 Uiso 1 1 calc R . . H2SC H 0.2988 -0.0332 0.0347 0.158 Uiso 1 1 calc R . . C1S C 0.2429(5) 0.0451(3) 0.07730(16) 0.0596(11) Uani 1 1 d U . . N1S N 0.2402(5) 0.1031(3) 0.08863(18) 0.0793(15) Uani 1 1 d U . . 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 0.0332(2) 0.0933(3) 0.0325(2) -0.00188(12) 0.01831(13) -0.00054(12) N1 0.0292(14) 0.0611(19) 0.0303(15) -0.0030(12) 0.0174(11) 0.0001(11) N2 0.0289(13) 0.0582(18) 0.0292(15) 0.0014(11) 0.0172(11) 0.0006(11) C1 0.0311(16) 0.070(2) 0.0344(19) 0.0001(15) 0.0105(14) -0.0029(14) C2 0.0336(17) 0.061(2) 0.0325(18) -0.0026(14) 0.0094(14) 0.0032(14) C3 0.0296(15) 0.059(2) 0.0299(17) 0.0003(13) 0.0125(13) -0.0020(13) C4 0.0420(18) 0.057(2) 0.0416(19) 0.0042(16) 0.0193(15) -0.0017(15) C5 0.0418(17) 0.056(2) 0.0430(19) -0.0035(16) 0.0213(15) 0.0008(15) C6 0.0410(17) 0.054(2) 0.0410(19) 0.0044(15) 0.0187(15) -0.0047(15) C7 0.0427(18) 0.050(2) 0.0425(19) -0.0046(15) 0.0202(15) 0.0003(14) C8 0.0283(16) 0.071(3) 0.0286(17) 0.0008(14) 0.0135(13) -0.0024(14) C9 0.0454(19) 0.066(3) 0.044(2) 0.0018(18) 0.0238(16) 0.0014(17) C10 0.0429(19) 0.068(3) 0.044(2) 0.0099(18) 0.0222(16) 0.0019(17) C11 0.0300(17) 0.072(3) 0.0271(17) 0.0004(14) 0.0126(13) -0.0027(14) C12 0.047(2) 0.068(3) 0.044(2) -0.0083(18) 0.0262(17) -0.0094(18) C13 0.047(2) 0.066(3) 0.046(2) -0.0043(18) 0.0257(17) -0.0109(18) C14 0.0311(17) 0.074(3) 0.0316(19) 0.0007(15) 0.0113(15) -0.0028(14) C15 0.0323(17) 0.070(3) 0.0330(19) 0.0027(14) 0.0135(15) -0.0039(14) C16 0.0307(16) 0.059(2) 0.0279(17) 0.0026(13) 0.0123(13) -0.0001(12) C17 0.0414(17) 0.052(2) 0.0410(19) -0.0058(15) 0.0203(14) -0.0014(15) C18 0.0402(17) 0.050(2) 0.0392(18) 0.0027(15) 0.0178(14) -0.0016(14) C19 0.0462(19) 0.053(2) 0.049(2) -0.0026(16) 0.0234(16) 0.0025(16) C20 0.0472(19) 0.053(2) 0.052(2) 0.0048(17) 0.0270(17) -0.0017(16) P1 0.0680(7) 0.0414(5) 0.0616(7) -0.0062(4) 0.0235(5) -0.0047(4) F1 0.143(4) 0.128(4) 0.132(4) 0.045(3) 0.003(3) 0.023(3) F2 0.151(4) 0.100(3) 0.113(3) -0.039(3) 0.026(3) -0.048(3) F3 0.123(3) 0.093(3) 0.135(4) -0.019(2) 0.082(3) -0.017(2) F4 0.109(3) 0.089(3) 0.137(4) -0.007(2) 0.073(3) -0.002(2) F5 0.135(4) 0.116(4) 0.167(5) -0.074(4) 0.031(3) -0.047(3) F6 0.129(4) 0.125(4) 0.202(6) 0.089(4) 0.029(4) 0.039(3) C2S 0.151(7) 0.055(3) 0.112(6) -0.005(3) 0.030(5) 0.010(4) C1S 0.065(3) 0.059(3) 0.057(2) -0.001(2) 0.025(2) 0.0040(19) N1S 0.081(3) 0.065(3) 0.095(4) -0.015(2) 0.039(3) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.152(3) . y Ag1 N2 2.149(3) 8_655 y N1 C5 1.332(5) . ? N1 C6 1.347(5) . ? N1S C1S 1.129(7) . ? N2 C19 1.340(5) . ? N2 C18 1.344(5) . ? N2 Ag1 2.149(3) 8_356 ? C1 C2 1.187(6) . ? C1 C8 1.436(5) . ? C1S C2S 1.466(8) . ? C2 C3 1.447(5) . ? C3 C7 1.383(5) . ? C3 C4 1.392(6) . ? C4 C5 1.395(5) . ? C6 C7 1.393(5) . ? C8 C13 1.394(6) . ? C8 C9 1.396(6) . ? C9 C10 1.388(6) . ? C10 C11 1.399(6) . ? C11 C12 1.399(6) . ? C11 C14 1.431(6) . ? C12 C13 1.394(6) . ? C14 C15 1.213(7) . ? C15 C16 1.423(5) . ? C16 C20 1.389(6) . ? C16 C17 1.401(5) . ? C17 C18 1.395(5) . ? C19 C20 1.393(5) . ? P1 F6 1.546(5) . ? P1 F2 1.568(4) . ? P1 F5 1.575(4) . ? P1 F1 1.584(5) . ? P1 F3 1.590(4) . ? P1 F4 1.592(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 N1 Ag1 N2 177.28(12) . 8_655. y C5 N1 C6 117.8(3) . . ? C5 N1 Ag1 119.9(3) . . ? C6 N1 Ag1 122.2(2) . . ? C19 N2 C18 117.4(3) . . ? C19 N2 Ag1 118.8(3) . 8_356 ? C18 N2 Ag1 123.8(2) . 8_356 ? C2 C1 C8 179.3(5) . . ? N1S C1S C2S 179.3(8) . . ? C1 C2 C3 178.9(5) . . ? C7 C3 C4 117.8(3) . . ? C7 C3 C2 122.1(3) . . ? C4 C3 C2 120.1(3) . . ? C3 C4 C5 118.9(4) . . ? N1 C5 C4 123.3(4) . . ? N1 C6 C7 122.2(4) . . ? C3 C7 C6 120.0(4) . . ? C13 C8 C9 119.3(4) . . ? C13 C8 C1 119.8(4) . . ? C9 C8 C1 120.9(4) . . ? C10 C9 C8 121.1(4) . . ? C9 C10 C11 119.7(4) . . ? C12 C11 C10 119.3(4) . . ? C12 C11 C14 120.6(4) . . ? C10 C11 C14 120.1(4) . . ? C13 C12 C11 120.7(4) . . ? C8 C13 C12 119.9(4) . . ? C15 C14 C11 178.1(5) . . ? C14 C15 C16 179.0(5) . . ? C20 C16 C17 117.4(4) . . ? C20 C16 C15 120.8(3) . . ? C17 C16 C15 121.7(3) . . ? C18 C17 C16 119.2(4) . . ? N2 C18 C17 123.1(3) . . ? N2 C19 C20 123.2(4) . . ? C16 C20 C19 119.6(4) . . ? F6 P1 F2 95.3(4) . . ? F6 P1 F5 85.1(4) . . ? F2 P1 F5 179.5(4) . . ? F6 P1 F1 178.2(3) . . ? F2 P1 F1 86.1(4) . . ? F5 P1 F1 93.5(4) . . ? F6 P1 F3 91.1(3) . . ? F2 P1 F3 89.9(3) . . ? F5 P1 F3 90.2(3) . . ? F1 P1 F3 90.0(3) . . ? F6 P1 F4 89.4(3) . . ? F2 P1 F4 89.5(3) . . ? F5 P1 F4 90.5(3) . . ? F1 P1 F4 89.5(3) . . ? F3 P1 F4 179.2(3) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 1.23 _refine_diff_density_min -0.81 _refine_diff_density_rms 0.09 #===END