# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Takafumi Kitazawa' _publ_contact_author_email KITAZAWA@CHEM.SCI.TOHO-U.AC.JP _publ_section_title ; A nobel spin crossover heterometallic FeIIAgI coordination polymer with the [Ag2(CN)3]- unit: crystallographic and magnetic study ; loop_ _publ_author_name 'Takafumi Kitazawa' 'Chikahide Kanadani' 'Takashi Kosone' 'Syota Ono' 'Toshiaki Saito' 'Yusuke Suzuki' # Attachment 'C2-c293K.cif' data_071203f_C2-c293K _database_code_depnum_ccdc_archive 'CCDC 726998' #TrackingRef 'C2-c293K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 Ag3 Fe N7' _chemical_formula_weight 723.86 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' Fe Fe 0.3463 0.8444 '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 12.7485(11) _cell_length_b 13.5326(11) _cell_length_c 14.0610(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.028(2) _cell_angle_gamma 90.00 _cell_volume 2381.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2758 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 3.047 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4617 _exptl_absorpt_correction_T_max 0.4617 _exptl_absorpt_process_details 'SADABS; sheldrick 1996' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8756 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 28.35 _reflns_number_total 2956 _reflns_number_gt 2872 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. This structure is possible to refine in both C2/c and Cc and it is a matter of debate whether to opt for pseudosymmetry and a lower symmetry or whether to model a single atom disorder in the higher symmetry with the application of positional and ADP restraints. We have decided to go for the first option. ; _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^)+(0.0293P)^2^+43.3387P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2956 _refine_ls_number_parameters 146 _refine_ls_number_restraints 206 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.1625 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 1.407 _refine_ls_restrained_S_all 1.362 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 1.0000 0.17056(8) 0.2500 0.0439(3) Uani 1 2 d SU . . Ag2 Ag 0.91871(7) 0.06197(6) 0.82484(5) 0.0547(3) Uani 1 1 d U . . Fe1 Fe 0.7500 0.2500 0.5000 0.0219(3) Uani 1 2 d SU . . N2 N 0.8551(6) 0.2012(5) 0.4083(5) 0.0359(15) Uani 1 1 d U . . C8 C 0.9053(7) 0.1844(7) 0.3508(7) 0.041(2) Uani 1 1 d U . . N1 N 0.6388(5) 0.1311(5) 0.4436(5) 0.0326(13) Uani 1 1 d U . . N3 N 0.8200(6) 0.1572(5) 0.6210(5) 0.0360(15) Uani 1 1 d U . . C1 C 0.6727(7) 0.0383(6) 0.4430(6) 0.0361(16) Uani 1 1 d U . . H5 H 0.7444 0.0258 0.4684 0.043 Uiso 1 1 calc R . . C9 C 0.8512(7) 0.1196(7) 0.6935(6) 0.0392(19) Uani 1 1 d U . . C2 C 0.6091(9) -0.0405(7) 0.4076(7) 0.047(2) Uani 1 1 d U . . C5 C 0.5354(7) 0.1478(7) 0.4068(6) 0.0375(17) Uani 1 1 d U . . H4 H 0.5105 0.2124 0.4075 0.045 Uiso 1 1 calc R . . C3 C 0.5022(8) -0.0205(8) 0.3709(6) 0.049(2) Uani 1 1 d U . . H2 H 0.4561 -0.0722 0.3481 0.059 Uiso 1 1 calc R . . C4 C 0.4628(7) 0.0751(8) 0.3676(6) 0.0431(19) Uani 1 1 d U . . C7 C 0.3498(8) 0.1001(10) 0.3268(8) 0.065(3) Uani 1 1 d U . . H10A H 0.3350 0.0864 0.2585 0.097 Uiso 1 1 calc R . . H10B H 0.3377 0.1689 0.3372 0.097 Uiso 1 1 calc R . . H10C H 0.3035 0.0610 0.3582 0.097 Uiso 1 1 calc R . . C6 C 0.6544(11) -0.1429(8) 0.4094(10) 0.072(3) Uani 1 1 d U . . H9A H 0.6651 -0.1603 0.3458 0.108 Uiso 1 1 calc R . . H9B H 0.6055 -0.1888 0.4296 0.108 Uiso 1 1 calc R . . H9C H 0.7215 -0.1453 0.4541 0.108 Uiso 1 1 calc R . . C10 C 0.9808(9) 0.0154(8) 0.9631(6) 0.065(12) Uani 0.50 1 d PU . . N4 N 0.9808(9) 0.0154(8) 0.9631(6) 0.062(10) Uani 0.50 1 d PU . . 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 0.0460(6) 0.0510(6) 0.0428(5) 0.000 0.0287(4) 0.000 Ag2 0.0628(5) 0.0631(5) 0.0300(4) 0.0204(3) -0.0117(3) -0.0109(4) Fe1 0.0221(7) 0.0264(7) 0.0175(6) 0.0036(5) 0.0042(5) 0.0017(6) N2 0.036(4) 0.037(4) 0.038(4) 0.002(3) 0.014(3) 0.002(3) C8 0.042(5) 0.041(5) 0.045(5) 0.003(4) 0.019(4) 0.002(4) N1 0.032(3) 0.039(3) 0.028(3) 0.004(3) 0.006(2) -0.003(3) N3 0.038(4) 0.038(4) 0.030(3) 0.006(3) 0.002(3) 0.004(3) C1 0.042(4) 0.039(4) 0.028(4) 0.002(3) 0.009(3) -0.002(3) C9 0.039(5) 0.044(5) 0.032(4) 0.014(3) 0.002(3) -0.002(4) C2 0.063(5) 0.044(4) 0.038(5) -0.007(4) 0.018(4) -0.011(4) C5 0.038(4) 0.049(5) 0.025(4) 0.005(3) 0.004(3) -0.002(3) C3 0.060(5) 0.057(5) 0.030(4) -0.005(4) 0.003(4) -0.026(4) C4 0.042(4) 0.066(5) 0.021(4) 0.005(4) 0.007(3) -0.019(4) C7 0.046(5) 0.095(9) 0.048(6) 0.003(6) -0.003(4) -0.019(5) C6 0.093(9) 0.047(5) 0.078(8) -0.015(6) 0.023(7) -0.008(5) C10 0.08(2) 0.06(2) 0.037(15) 0.025(17) -0.014(19) -0.04(2) N4 0.077(18) 0.072(19) 0.028(12) 0.014(14) -0.013(15) -0.037(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C8 2.039(8) . ? Ag1 C8 2.039(8) 2_755 ? Ag2 C9 2.037(8) . ? Ag2 C10 2.053(8) . ? Ag2 Ag2 3.2240(18) 2_756 ? Fe1 N2 2.134(7) 7_656 ? Fe1 N2 2.134(7) . ? Fe1 N3 2.165(7) . ? Fe1 N3 2.165(7) 7_656 ? Fe1 N1 2.191(7) . ? Fe1 N1 2.191(7) 7_656 ? N2 C8 1.146(11) . ? N1 C1 1.328(11) . ? N1 C5 1.340(11) . ? N3 C9 1.141(10) . ? C1 C2 1.374(12) . ? C1 H5 0.9300 . ? C2 C3 1.389(15) . ? C2 C6 1.500(15) . ? C5 C4 1.390(12) . ? C5 H4 0.9300 . ? C3 C4 1.385(15) . ? C3 H2 0.9300 . ? C4 C7 1.485(14) . ? C7 H10A 0.9600 . ? C7 H10B 0.9600 . ? C7 H10C 0.9600 . ? C6 H9A 0.9600 . ? C6 H9B 0.9600 . ? C6 H9C 0.9600 . ? C10 N4 1.139(16) 5_757 ? C10 C10 1.139(16) 5_757 ? 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 C8 Ag1 C8 169.5(5) . 2_755 ? C9 Ag2 C10 174.5(4) . . ? C9 Ag2 Ag2 67.7(3) . 2_756 ? C10 Ag2 Ag2 116.0(3) . 2_756 ? N2 Fe1 N2 180.000(1) 7_656 . ? N2 Fe1 N3 85.2(3) 7_656 . ? N2 Fe1 N3 94.8(3) . . ? N2 Fe1 N3 94.8(3) 7_656 7_656 ? N2 Fe1 N3 85.2(3) . 7_656 ? N3 Fe1 N3 180.0(3) . 7_656 ? N2 Fe1 N1 90.5(3) 7_656 . ? N2 Fe1 N1 89.5(3) . . ? N3 Fe1 N1 89.9(3) . . ? N3 Fe1 N1 90.1(3) 7_656 . ? N2 Fe1 N1 89.5(3) 7_656 7_656 ? N2 Fe1 N1 90.5(3) . 7_656 ? N3 Fe1 N1 90.1(3) . 7_656 ? N3 Fe1 N1 89.9(3) 7_656 7_656 ? N1 Fe1 N1 180.0(2) . 7_656 ? C8 N2 Fe1 171.0(7) . . ? N2 C8 Ag1 173.6(8) . . ? C1 N1 C5 117.1(8) . . ? C1 N1 Fe1 120.5(6) . . ? C5 N1 Fe1 122.4(6) . . ? C9 N3 Fe1 169.1(7) . . ? N1 C1 C2 124.4(9) . . ? N1 C1 H5 117.8 . . ? C2 C1 H5 117.8 . . ? N3 C9 Ag2 174.5(8) . . ? C1 C2 C3 116.9(9) . . ? C1 C2 C6 120.8(10) . . ? C3 C2 C6 122.3(9) . . ? N1 C5 C4 124.3(9) . . ? N1 C5 H4 117.8 . . ? C4 C5 H4 117.8 . . ? C4 C3 C2 121.2(9) . . ? C4 C3 H2 119.4 . . ? C2 C3 H2 119.4 . . ? C3 C4 C5 116.0(9) . . ? C3 C4 C7 122.9(9) . . ? C5 C4 C7 121.0(10) . . ? C4 C7 H10A 109.5 . . ? C4 C7 H10B 109.5 . . ? H10A C7 H10B 109.5 . . ? C4 C7 H10C 109.5 . . ? H10A C7 H10C 109.5 . . ? H10B C7 H10C 109.5 . . ? C2 C6 H9A 109.5 . . ? C2 C6 H9B 109.5 . . ? H9A C6 H9B 109.5 . . ? C2 C6 H9C 109.5 . . ? H9A C6 H9C 109.5 . . ? H9B C6 H9C 109.5 . . ? N4 C10 C10 0.0(10) 5_757 5_757 ? N4 C10 Ag2 175.1(17) 5_757 . ? C10 C10 Ag2 175.1(17) 5_757 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.069 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.164 # Attachment 'Cc293K.cif' data_071203f_Cc293K _database_code_depnum_ccdc_archive 'CCDC 726999' #TrackingRef 'Cc293K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 Ag3 Fe N7' _chemical_formula_weight 723.86 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.7485(11) _cell_length_b 13.5326(11) _cell_length_c 14.0610(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.028(2) _cell_angle_gamma 90.00 _cell_volume 2381.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2758 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 3.047 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4617 _exptl_absorpt_correction_T_max 0.4617 _exptl_absorpt_process_details 'SADABS; sheldrick 1996' _exptl_special_details ; high-spin state ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8756 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 28.35 _reflns_number_total 4519 _reflns_number_gt 4313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. This structure is possible to refine in both Cc and C2/c and it is a matter of debate whether to opt for pseudosymmetry and a lower symmetry or whether to model a single atom disorder in the higher symmetry with the application of positional and ADP restraints. We have decided to go for the first option. ; _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^)+(0.0315P)^2^+24.8016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.33(10) _refine_ls_number_reflns 4519 _refine_ls_number_parameters 258 _refine_ls_number_restraints 552 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 1.250 _refine_ls_restrained_S_all 1.184 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C19 C -0.046(2) 0.9883(18) -0.1291(12) 0.0359(11) Uani 0.60(3) 1 d PDU A 1 N7 N -0.0794(15) 1.0195(17) -0.2048(12) 0.0338(16) Uani 0.60(3) 1 d PDU A 1 C20 C -0.046(3) 0.997(2) -0.2213(17) 0.0359(11) Uani 0.40(3) 1 d PDU A 2 N8 N -0.012(2) 0.973(2) -0.1449(18) 0.0338(16) Uani 0.40(3) 1 d PDU A 2 C16 C 0.3460(12) 0.6898(10) 0.1718(8) 0.0359(11) Uani 1 1 d U . . C17 C 0.2915(13) 0.6218(12) 0.5211(12) 0.046(3) Uani 1 1 d U . . N5 N 0.2671(12) 0.6582(9) 0.4523(10) 0.038(2) Uani 1 1 d U . . Ag3 Ag -0.13554(9) 1.06169(13) -0.34477(7) 0.0700(5) Uani 1 1 d DU . . N2 N 0.0814(8) 0.6318(7) 0.2736(8) 0.039(2) Uani 1 1 d DU . . Ag1 Ag -0.05545(18) 0.82936(5) 0.57974(14) 0.0461(2) Uani 1 1 d U . . Ag2 Ag 0.02701(4) 0.93775(9) 0.00556(4) 0.0452(3) Uani 1 1 d DU . . Fe1 Fe 0.1965(2) 0.75004(17) 0.32993(18) 0.0243(2) Uani 1 1 d U A . C18 C 0.0365(12) 0.8200(10) 0.4708(8) 0.0359(11) Uani 1 1 d U A . N1 N 0.3043(8) 0.8690(7) 0.3862(7) 0.0302(19) Uani 1 1 d DU . . N3 N 0.1275(12) 0.8445(9) 0.2106(9) 0.036(2) Uani 1 1 d U . . C4 C 0.3352(12) 1.0422(9) 0.4190(11) 0.049(3) Uani 1 1 d DU . . C5 C 0.2708(11) 0.9627(8) 0.3857(10) 0.040(3) Uani 1 1 d DU . . H5 H 0.1990 0.9752 0.3611 0.048 Uiso 1 1 calc R . . C2 C 0.4810(9) 0.9257(9) 0.4614(8) 0.042(3) Uani 1 1 d DU . . C1 C 0.4081(8) 0.8536(9) 0.4236(7) 0.040(3) Uani 1 1 d DU . . H1 H 0.4330 0.7889 0.4241 0.048 Uiso 1 1 calc R . . C8 C -0.0215(9) 0.6496(8) 0.2364(7) 0.039(3) Uani 1 1 d DU . . H8 H -0.0464 0.7142 0.2366 0.047 Uiso 1 1 calc R . . C9 C -0.0927(10) 0.5763(9) 0.1977(9) 0.050(3) Uani 1 1 d DU . . C10 C -0.0540(10) 0.4803(9) 0.2014(11) 0.045(3) Uani 1 1 d DU . . H10 H -0.1008 0.4285 0.1808 0.054 Uiso 1 1 calc R . . C15 C 0.0888(13) 0.8818(11) 0.1345(10) 0.0359(11) Uani 1 1 d U A . C3 C 0.4404(12) 1.0209(9) 0.4593(12) 0.058(4) Uani 1 1 d DU . . H3 H 0.4853 1.0721 0.4859 0.070 Uiso 1 1 calc R . . C13 C -0.2054(16) 0.6028(19) 0.1560(15) 0.066(5) Uani 1 1 d DU . . H13A H -0.2278 0.5688 0.0956 0.098 Uiso 1 1 calc R . . H13B H -0.2106 0.6728 0.1452 0.098 Uiso 1 1 calc R . . H13C H -0.2505 0.5840 0.2004 0.098 Uiso 1 1 calc R . . C7 C 0.291(2) 1.1431(14) 0.4185(18) 0.079(6) Uani 1 1 d DU . . H7A H 0.3061 1.1699 0.4829 0.118 Uiso 1 1 calc R . . H7B H 0.2145 1.1407 0.3963 0.118 Uiso 1 1 calc R . . H7C H 0.3219 1.1843 0.3759 0.118 Uiso 1 1 calc R . . C14 C 0.099(2) 0.3564(14) 0.2384(17) 0.068(5) Uani 1 1 d DU . . H14A H 0.0437 0.3092 0.2422 0.102 Uiso 1 1 calc R . . H14B H 0.1550 0.3500 0.2943 0.102 Uiso 1 1 calc R . . H14C H 0.1272 0.3446 0.1809 0.102 Uiso 1 1 calc R . . C6 C 0.5952(16) 0.903(2) 0.5018(13) 0.068(5) Uani 1 1 d DU . . H6A H 0.6382 0.9602 0.4950 0.102 Uiso 1 1 calc R . . H6B H 0.6181 0.8487 0.4672 0.102 Uiso 1 1 calc R . . H6C H 0.6030 0.8865 0.5691 0.102 Uiso 1 1 calc R . . C12 C 0.1167(10) 0.5390(8) 0.2722(10) 0.037(3) Uani 1 1 d DU . . H12 H 0.1884 0.5266 0.2976 0.044 Uiso 1 1 calc R . . C11 C 0.0527(11) 0.4603(9) 0.2349(11) 0.046(3) Uani 1 1 d DU . . N6 N 0.0890(9) 0.8036(10) 0.4201(8) 0.0338(16) Uani 1 1 d U . . N4 N 0.2985(11) 0.7039(8) 0.2358(9) 0.041(2) 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 C19 0.039(3) 0.042(3) 0.028(2) 0.011(2) 0.010(2) 0.003(2) N7 0.022(4) 0.058(4) 0.022(3) 0.003(3) 0.005(2) -0.007(3) C20 0.039(3) 0.042(3) 0.028(2) 0.011(2) 0.010(2) 0.003(2) N8 0.022(4) 0.058(4) 0.022(3) 0.003(3) 0.005(2) -0.007(3) C16 0.039(3) 0.042(3) 0.028(2) 0.011(2) 0.010(2) 0.003(2) C17 0.034(7) 0.050(7) 0.047(6) 0.021(5) -0.011(5) 0.000(5) N5 0.034(7) 0.041(5) 0.035(5) 0.006(4) -0.006(4) -0.002(4) Ag3 0.0751(11) 0.0856(10) 0.0411(7) 0.0147(7) -0.0099(7) 0.0016(8) N2 0.038(5) 0.046(4) 0.029(5) 0.006(4) -0.004(4) -0.006(4) Ag1 0.0473(4) 0.0549(4) 0.0442(4) 0.0004(6) 0.0286(3) 0.0006(7) Ag2 0.0546(7) 0.0502(5) 0.0227(4) 0.0239(4) -0.0130(4) -0.0199(6) Fe1 0.0232(5) 0.0311(5) 0.0188(5) 0.0033(4) 0.0047(4) 0.0023(4) C18 0.039(3) 0.042(3) 0.028(2) 0.011(2) 0.010(2) 0.003(2) N1 0.026(4) 0.038(4) 0.031(5) 0.000(4) 0.016(4) 0.001(3) N3 0.042(7) 0.044(5) 0.024(4) 0.009(4) 0.009(4) 0.013(4) C4 0.074(9) 0.042(5) 0.029(7) -0.009(5) 0.009(7) -0.009(5) C5 0.049(8) 0.040(5) 0.032(7) 0.004(5) 0.009(6) -0.002(4) C2 0.039(6) 0.074(7) 0.019(6) -0.003(5) 0.018(5) -0.019(5) C1 0.038(6) 0.054(6) 0.027(7) 0.010(5) 0.006(6) -0.006(5) C8 0.038(6) 0.049(6) 0.029(7) 0.000(5) 0.003(6) 0.002(4) C9 0.039(7) 0.069(7) 0.036(7) 0.013(6) -0.008(6) -0.019(5) C10 0.046(6) 0.059(6) 0.032(7) -0.010(6) 0.012(6) -0.025(5) C15 0.039(3) 0.042(3) 0.028(2) 0.011(2) 0.010(2) 0.003(2) C3 0.076(9) 0.058(6) 0.036(8) 0.002(7) -0.002(8) -0.028(6) C13 0.039(7) 0.093(12) 0.065(12) 0.011(10) 0.009(8) -0.015(7) C7 0.110(16) 0.041(7) 0.091(16) -0.027(9) 0.036(13) -0.008(8) C14 0.084(14) 0.052(7) 0.066(12) -0.003(8) 0.009(11) -0.006(7) C6 0.051(8) 0.109(14) 0.036(9) 0.005(9) -0.010(8) -0.027(7) C12 0.032(7) 0.050(5) 0.029(6) -0.006(5) 0.008(6) 0.001(4) C11 0.055(7) 0.049(6) 0.040(8) -0.002(5) 0.022(7) -0.011(5) N6 0.022(4) 0.058(4) 0.022(3) 0.003(3) 0.005(2) -0.007(3) N4 0.053(6) 0.027(4) 0.047(5) 0.007(4) 0.023(5) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C19 N7 1.147(19) . ? C19 Ag2 2.063(15) . ? N7 Ag3 2.043(17) . ? C20 N8 1.13(3) . ? C20 Ag3 2.079(16) . ? N8 Ag2 2.13(2) . ? C16 N4 1.192(17) . ? C16 Ag1 1.986(13) 4_564 ? C17 N5 1.077(19) . ? C17 Ag3 2.101(14) 3_546 ? N5 Fe1 2.173(13) . ? Ag3 C17 2.101(14) 3_454 ? Ag3 Ag2 3.2237(13) 2_574 ? N2 C12 1.336(10) . ? N2 C8 1.338(8) . ? N2 Fe1 2.213(10) . ? Ag1 C16 1.986(13) 4_465 ? Ag1 C18 2.104(13) . ? Ag2 C15 1.983(14) . ? Ag2 Ag3 3.2237(13) 2_575 ? Fe1 N4 2.119(12) . ? Fe1 N3 2.159(12) . ? Fe1 N6 2.163(12) . ? Fe1 N1 2.165(10) . ? C18 N6 1.089(17) . ? N1 C5 1.338(11) . ? N1 C1 1.344(8) . ? N3 C15 1.200(18) . ? C4 C5 1.380(13) . ? C4 C3 1.382(14) . ? C4 C7 1.48(2) . ? C5 H5 0.9300 . ? C2 C1 1.383(8) . ? C2 C3 1.387(9) . ? C2 C6 1.49(2) . ? C1 H1 0.9300 . ? C8 C9 1.384(8) . ? C8 H8 0.9300 . ? C9 C10 1.386(8) . ? C9 C13 1.49(2) . ? C10 C11 1.378(13) . ? C10 H10 0.9300 . ? C3 H3 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C14 C11 1.52(2) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C12 C11 1.382(13) . ? C12 H12 0.9300 . ? 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 N7 C19 Ag2 174.4(19) . . ? C19 N7 Ag3 174.3(16) . . ? N8 C20 Ag3 165(3) . . ? C20 N8 Ag2 170(2) . . ? N4 C16 Ag1 171.4(14) . 4_564 ? N5 C17 Ag3 170.3(15) . 3_546 ? C17 N5 Fe1 167.8(15) . . ? N7 Ag3 C20 16.8(9) . . ? N7 Ag3 C17 170.6(8) . 3_454 ? C20 Ag3 C17 172.1(11) . 3_454 ? N7 Ag3 Ag2 118.6(5) . 2_574 ? C20 Ag3 Ag2 103.2(10) . 2_574 ? C17 Ag3 Ag2 69.0(5) 3_454 2_574 ? C12 N2 C8 118.1(11) . . ? C12 N2 Fe1 118.9(8) . . ? C8 N2 Fe1 122.9(8) . . ? C16 Ag1 C18 167.7(4) 4_465 . ? C15 Ag2 C19 175.7(9) . . ? C15 Ag2 N8 165.7(10) . . ? C19 Ag2 N8 15.3(8) . . ? C15 Ag2 Ag3 66.2(4) . 2_575 ? C19 Ag2 Ag3 111.3(7) . 2_575 ? N8 Ag2 Ag3 126.1(8) . 2_575 ? N4 Fe1 N3 84.1(5) . . ? N4 Fe1 N6 176.7(6) . . ? N3 Fe1 N6 92.7(5) . . ? N4 Fe1 N1 91.4(5) . . ? N3 Fe1 N1 88.8(5) . . ? N6 Fe1 N1 88.0(4) . . ? N4 Fe1 N5 96.6(5) . . ? N3 Fe1 N5 178.6(7) . . ? N6 Fe1 N5 86.6(5) . . ? N1 Fe1 N5 89.9(4) . . ? N4 Fe1 N2 90.5(5) . . ? N3 Fe1 N2 90.4(5) . . ? N6 Fe1 N2 90.0(5) . . ? N1 Fe1 N2 177.9(5) . . ? N5 Fe1 N2 90.9(4) . . ? N6 C18 Ag1 170.5(12) . . ? C5 N1 C1 116.0(11) . . ? C5 N1 Fe1 121.6(8) . . ? C1 N1 Fe1 122.4(7) . . ? C15 N3 Fe1 168.2(12) . . ? C5 C4 C3 116.4(12) . . ? C5 C4 C7 121.0(16) . . ? C3 C4 C7 122.4(15) . . ? N1 C5 C4 124.7(12) . . ? N1 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? C1 C2 C3 115.3(12) . . ? C1 C2 C6 122.6(14) . . ? C3 C2 C6 122.1(14) . . ? N1 C1 C2 125.5(12) . . ? N1 C1 H1 117.3 . . ? C2 C1 H1 117.3 . . ? N2 C8 C9 123.0(11) . . ? N2 C8 H8 118.5 . . ? C9 C8 H8 118.5 . . ? C8 C9 C10 117.1(11) . . ? C8 C9 C13 119.5(14) . . ? C10 C9 C13 123.4(13) . . ? C11 C10 C9 121.2(11) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? N3 C15 Ag2 177.2(13) . . ? C4 C3 C2 122.1(12) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C12 C11 123.6(12) . . ? N2 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? C10 C11 C12 116.8(11) . . ? C10 C11 C14 122.9(14) . . ? C12 C11 C14 120.1(14) . . ? C18 N6 Fe1 171.5(12) . . ? C16 N4 Fe1 168.4(11) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.243 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.151 # Attachment 'C2-c80K.cif' data_071203f_C2-c80K _database_code_depnum_ccdc_archive 'CCDC 727000' #TrackingRef 'C2-c80K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 Ag3 Fe N7' _chemical_formula_weight 723.86 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' Fe Fe 0.3463 0.8444 '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 12.4686(10) _cell_length_b 13.0951(10) _cell_length_c 13.6139(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.954(2) _cell_angle_gamma 90.00 _cell_volume 2189.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used 2258 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 3.314 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4364 _exptl_absorpt_correction_T_max 0.4364 _exptl_absorpt_process_details 'SADABS; sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 80(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7906 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.30 _reflns_number_total 2728 _reflns_number_gt 2711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. This structure is possible to refine in both C2/c and Cc and it is a matter of debate whether to opt for pseudosymmetry and a lower symmetry or whether to model a single atom disorder in the higher symmetry with the application of positional and ADP restraints. We have decided to go for the first option. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+271.8411P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2728 _refine_ls_number_parameters 110 _refine_ls_number_restraints 206 _refine_ls_R_factor_all 0.1131 _refine_ls_R_factor_gt 0.1121 _refine_ls_wR_factor_ref 0.2213 _refine_ls_wR_factor_gt 0.2209 _refine_ls_goodness_of_fit_ref 1.533 _refine_ls_restrained_S_all 1.477 _refine_ls_shift/su_max 0.195 _refine_ls_shift/su_mean 0.018 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag2 Ag 0.5000 0.82902(3) 0.7500 0.00783(9) Uani 1 2 d SU . . Ag1 Ag 0.41429(3) 0.93945(2) 1.31866(2) 0.00939(7) Uani 1 1 d U . . Fe1 Fe 0.2500 0.7500 1.0000 0.00379(17) Uani 1 2 d SU . . N1 N 0.1466(3) 0.8613(3) 0.9473(2) 0.0084(5) Uani 1 1 d U . . N2 N 0.3134(3) 0.8362(3) 1.1106(2) 0.0067(3) Uani 1 1 d U . . C4 C 0.1142(3) 1.0387(3) 0.9068(3) 0.0111(8) Uani 1 1 d U . . C1 C 0.0415(3) 0.8430(3) 0.9113(3) 0.0062(8) Uani 1 1 d U . . H1 H 0.0164 0.7746 0.9133 0.007 Uiso 1 1 calc R . . C2 C -0.0330(3) 0.9166(3) 0.8714(3) 0.0096(8) Uani 1 1 d U . . C5 C 0.1809(3) 0.9585(3) 0.9445(3) 0.0063(7) Uani 1 1 d U . . H5 H 0.2552 0.9729 0.9700 0.008 Uiso 1 1 calc R . . C3 C 0.0046(3) 1.0168(3) 0.8723(3) 0.0084(5) Uani 1 1 d U . . H3 H -0.0446 1.0705 0.8494 0.010 Uiso 1 1 calc R . . C7 C 0.1607(4) 1.1444(3) 0.9067(3) 0.0157(10) Uani 1 1 d U . . H7A H 0.2349 1.1448 0.9449 0.024 Uiso 1 1 calc R . . H7B H 0.1153 1.1919 0.9372 0.024 Uiso 1 1 calc R . . H7C H 0.1623 1.1656 0.8379 0.024 Uiso 1 1 calc R . . N3 N 0.3492(3) 0.7954(3) 0.9145(2) 0.0067(3) Uani 1 1 d U . . C9 C 0.4014(3) 0.8134(3) 0.8549(3) 0.0067(3) Uani 1 1 d U . . C8 C 0.3452(3) 0.8794(3) 1.1838(3) 0.0067(3) Uani 1 1 d U . . C6 C -0.1480(3) 0.8903(3) 0.8304(3) 0.0113(9) Uani 1 1 d U . . H6A H -0.1580 0.8880 0.7575 0.017 Uiso 1 1 calc R . . H6B H -0.1963 0.9422 0.8510 0.017 Uiso 1 1 calc R . . H6C H -0.1655 0.8235 0.8559 0.017 Uiso 1 1 calc R . . C10 C 0.4794(3) 0.9850(3) 1.4626(3) 0.0067(3) Uani 0.50 1 d PU . . N4 N 0.4794(3) 0.9850(3) 1.4626(3) 0.0067(3) Uani 0.50 1 d PU . . 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 Ag2 0.00800(16) 0.00856(17) 0.00800(16) 0.000 0.00439(13) 0.000 Ag1 0.01050(12) 0.01180(12) 0.00438(11) -0.00406(11) -0.00297(9) -0.00019(12) Fe1 0.0030(3) 0.0074(3) 0.0007(3) -0.0010(3) -0.0006(2) -0.0004(3) N1 0.0114(8) 0.0099(9) 0.0036(9) -0.0030(9) 0.0005(8) 0.0011(8) N2 0.0080(6) 0.0043(6) 0.0065(6) 0.0032(5) -0.0024(5) 0.0018(5) C4 0.0119(14) 0.0136(14) 0.0070(15) 0.0001(14) -0.0010(13) 0.0024(12) C1 0.0067(12) 0.0053(13) 0.0071(14) -0.0030(13) 0.0025(11) -0.0031(11) C2 0.0108(13) 0.0121(15) 0.0068(15) -0.0021(14) 0.0045(12) 0.0017(11) C5 0.0073(13) 0.0091(12) 0.0029(13) 0.0006(12) 0.0022(11) -0.0035(11) C3 0.0114(8) 0.0099(9) 0.0036(9) -0.0030(9) 0.0005(8) 0.0011(8) C7 0.0143(18) 0.0110(14) 0.020(2) 0.0002(16) -0.0018(16) 0.0009(14) N3 0.0080(6) 0.0043(6) 0.0065(6) 0.0032(5) -0.0024(5) 0.0018(5) C9 0.0080(6) 0.0043(6) 0.0065(6) 0.0032(5) -0.0024(5) 0.0018(5) C8 0.0080(6) 0.0043(6) 0.0065(6) 0.0032(5) -0.0024(5) 0.0018(5) C6 0.0121(14) 0.0090(16) 0.0124(17) 0.0081(15) 0.0007(13) -0.0011(13) C10 0.0080(6) 0.0043(6) 0.0065(6) 0.0032(5) -0.0024(5) 0.0018(5) N4 0.0080(6) 0.0043(6) 0.0065(6) 0.0032(5) -0.0024(5) 0.0018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag2 C9 2.049(4) . ? Ag2 C9 2.049(4) 2_656 ? Ag1 C8 2.045(4) . ? Ag1 C10 2.075(3) . ? Ag1 Ag1 3.0732(7) 2_657 ? Fe1 N3 1.932(4) . ? Fe1 N3 1.932(4) 7_567 ? Fe1 N2 1.937(3) . ? Fe1 N2 1.937(3) 7_567 ? Fe1 N1 1.996(3) . ? Fe1 N1 1.996(3) 7_567 ? N1 C1 1.339(5) . ? N1 C5 1.345(5) . ? N2 C8 1.155(5) . ? C4 C5 1.382(6) . ? C4 C3 1.396(6) . ? C4 C7 1.500(6) . ? C1 C2 1.383(5) . ? C1 H1 0.9500 . ? C2 C3 1.392(6) . ? C2 C6 1.486(6) . ? C5 H5 0.9500 . ? C3 H3 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? N3 C9 1.150(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C10 N4 1.129(7) 5_678 ? C10 C10 1.129(7) 5_678 ? 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 C9 Ag2 C9 168.5(2) . 2_656 ? C8 Ag1 C10 173.46(15) . . ? C8 Ag1 Ag1 71.54(12) . 2_657 ? C10 Ag1 Ag1 112.00(11) . 2_657 ? N3 Fe1 N3 180.000(1) . 7_567 ? N3 Fe1 N2 94.07(14) . . ? N3 Fe1 N2 85.93(14) 7_567 . ? N3 Fe1 N2 85.93(14) . 7_567 ? N3 Fe1 N2 94.07(14) 7_567 7_567 ? N2 Fe1 N2 180.000(1) . 7_567 ? N3 Fe1 N1 89.98(14) . . ? N3 Fe1 N1 90.02(14) 7_567 . ? N2 Fe1 N1 90.30(13) . . ? N2 Fe1 N1 89.70(13) 7_567 . ? N3 Fe1 N1 90.02(14) . 7_567 ? N3 Fe1 N1 89.98(14) 7_567 7_567 ? N2 Fe1 N1 89.70(13) . 7_567 ? N2 Fe1 N1 90.30(13) 7_567 7_567 ? N1 Fe1 N1 180.000(1) . 7_567 ? C1 N1 C5 117.1(3) . . ? C1 N1 Fe1 122.1(3) . . ? C5 N1 Fe1 120.8(3) . . ? C8 N2 Fe1 171.5(3) . . ? C5 C4 C3 117.3(4) . . ? C5 C4 C7 119.6(4) . . ? C3 C4 C7 123.1(4) . . ? N1 C1 C2 124.5(4) . . ? N1 C1 H1 117.7 . . ? C2 C1 H1 117.7 . . ? C1 C2 C3 116.8(4) . . ? C1 C2 C6 121.7(4) . . ? C3 C2 C6 121.5(4) . . ? N1 C5 C4 123.8(4) . . ? N1 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 N3 Fe1 171.1(3) . . ? N3 C9 Ag2 173.7(3) . . ? N2 C8 Ag1 172.4(3) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C10 C10 0.0(2) 5_678 5_678 ? N4 C10 Ag1 174.2(5) 5_678 . ? C10 C10 Ag1 174.2(5) 5_678 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.241 _refine_diff_density_min -4.849 _refine_diff_density_rms 0.385 # Attachment 'Cc80K.cif' data_071203f_Cc80K _database_code_depnum_ccdc_archive 'CCDC 727001' #TrackingRef 'Cc80K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 Ag3 Fe N7' _chemical_formula_weight 723.86 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 12.4686(10) _cell_length_b 13.0951(10) _cell_length_c 13.6139(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.954(2) _cell_angle_gamma 90.00 _cell_volume 2189.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 80(2) _cell_measurement_reflns_used 2258 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 3.314 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4364 _exptl_absorpt_correction_T_max 0.4364 _exptl_absorpt_process_details 'SADABS; sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 80(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7906 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 28.30 _reflns_number_total 4124 _reflns_number_gt 4091 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+221.9730P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.44(17) _refine_ls_number_reflns 4124 _refine_ls_number_parameters 240 _refine_ls_number_restraints 429 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_ref 0.1890 _refine_ls_wR_factor_gt 0.1886 _refine_ls_goodness_of_fit_ref 1.366 _refine_ls_restrained_S_all 1.299 _refine_ls_shift/su_max 6.467 _refine_ls_shift/su_mean 0.204 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N8 N 0.496(3) 0.978(3) 0.524(2) 0.018(3) Uani 0.16(2) 1 d PU A 1 C20 C 0.466(3) 1.019(3) 0.447(3) 0.012(3) Uani 0.16(2) 1 d PU A 1 N7 N 0.4511(5) 1.0198(4) 0.4493(4) 0.0089(11) Uani 0.84(2) 1 d PU A 2 C19 C 0.4939(7) 0.9927(6) 0.5269(6) 0.0190(15) Uani 0.84(2) 1 d PU A 2 N6 N 0.2843(3) 1.1622(3) 0.0925(3) 0.0054(6) Uani 1 1 d U . . N3 N 1.1255(3) 0.7078(3) 0.5682(3) 0.0054(6) Uani 1 1 d U . . C15 C 1.0725(4) 0.6836(4) 0.6316(4) 0.0123(11) Uani 1 1 d U . . C18 C 0.3240(5) 1.1205(4) 0.1728(4) 0.0117(12) Uani 1 1 d U A . Ag3 Ag 0.38956(2) 1.06065(3) 0.30048(2) 0.00882(8) Uani 1 1 d U . . Ag2 Ag 0.56065(4) 0.93967(4) 0.66312(3) 0.02201(12) Uani 1 1 d U . . Ag1 Ag 0.97890(6) 0.67106(2) 0.73071(5) 0.01200(7) Uani 1 1 d U . . Fe1 Fe 0.72438(10) 0.75562(7) 0.98514(8) 0.00616(14) Uani 1 1 d U . . N2 N 0.8250(4) 0.8659(3) 1.0381(3) 0.0082(5) Uani 1 1 d U . . N1 N 0.6181(4) 0.6430(3) 0.9338(3) 0.0082(5) Uani 1 1 d U . . N4 N 0.6579(4) 0.8341(4) 0.8722(4) 0.0126(10) Uani 1 1 d U . . C2 C 0.4410(5) 0.5824(4) 0.8501(4) 0.0123(8) Uani 1 1 d U . . C1 C 0.5162(4) 0.6556(4) 0.8902(4) 0.0102(4) Uani 1 1 d U . . H1 H 0.4908 0.7241 0.8857 0.012 Uiso 1 1 calc R . . C9 C 1.0048(4) 0.9164(4) 1.1064(4) 0.0108(7) Uani 1 1 d U . . C8 C 0.9342(4) 0.8419(4) 1.0657(4) 0.0102(4) Uani 1 1 d U . . H8 H 0.9595 0.7747 1.0565 0.012 Uiso 1 1 calc R . . C3 C 0.4765(5) 0.4820(4) 0.8482(4) 0.0137(11) Uani 1 1 d U . . H3 H 0.4285 0.4301 0.8180 0.016 Uiso 1 1 calc R . . C4 C 0.5861(5) 0.4577(4) 0.8923(4) 0.0123(8) Uani 1 1 d U . . C6 C 0.3259(5) 0.6079(4) 0.8135(4) 0.0158(7) Uani 1 1 d U . . H6A H 0.3027 0.6615 0.8555 0.024 Uiso 1 1 calc R . . H6B H 0.2809 0.5469 0.8163 0.024 Uiso 1 1 calc R . . H6C H 0.3175 0.6321 0.7445 0.024 Uiso 1 1 calc R . . C5 C 0.6593(5) 0.5381(4) 0.9305(4) 0.0102(4) Uani 1 1 d U . . H5 H 0.7341 0.5238 0.9536 0.012 Uiso 1 1 calc R . . C10 C 0.9649(5) 1.0169(4) 1.1032(4) 0.0134(10) Uani 1 1 d U . . H10 H 1.0140 1.0723 1.1196 0.016 Uiso 1 1 calc R . . C7 C 0.6436(5) 0.3547(4) 0.8911(5) 0.0185(8) Uani 1 1 d U . . H7A H 0.6501 0.3371 0.8224 0.028 Uiso 1 1 calc R . . H7B H 0.6012 0.3019 0.9183 0.028 Uiso 1 1 calc R . . H7C H 0.7164 0.3590 0.9319 0.028 Uiso 1 1 calc R . . N5 N 0.8236(4) 0.7031(4) 0.8961(4) 0.0136(9) Uani 1 1 d U . . C17 C 0.8731(5) 0.6888(5) 0.8394(5) 0.0207(12) Uani 1 1 d U A . C16 C 0.6319(5) 0.8792(4) 0.8055(4) 0.0156(12) Uani 1 1 d U A . C12 C 0.7976(5) 0.9553(4) 1.0410(4) 0.0102(4) Uani 1 1 d U . . H12 H 0.7237 0.9696 1.0139 0.012 Uiso 1 1 calc R . . C11 C 0.8577(4) 1.0352(4) 1.0771(4) 0.0108(7) Uani 1 1 d U . . C13 C 1.1239(5) 0.8880(4) 1.1528(4) 0.0158(7) Uani 1 1 d U . . H13A H 1.1744 0.9263 1.1190 0.024 Uiso 1 1 calc R . . H13B H 1.1351 0.8146 1.1447 0.024 Uiso 1 1 calc R . . H13C H 1.1373 0.9053 1.2239 0.024 Uiso 1 1 calc R . . C14 C 0.8211(5) 1.1437(4) 1.0771(5) 0.0185(8) Uani 1 1 d U . . H14A H 0.8224 1.1663 1.1459 0.028 Uiso 1 1 calc R . . H14B H 0.7468 1.1493 1.0396 0.028 Uiso 1 1 calc R . . H14C H 0.8700 1.1867 1.0458 0.028 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 N8 0.016(6) 0.021(5) 0.0159(19) 0.002(2) -0.002(3) 0.004(5) C20 0.010(6) 0.009(5) 0.0145(19) 0.001(2) -0.003(3) -0.003(5) N7 0.014(2) 0.0044(19) 0.0099(14) -0.0007(15) 0.0058(16) -0.0031(18) C19 0.018(3) 0.020(3) 0.0181(16) 0.0011(19) 0.000(2) 0.010(2) N6 0.0059(12) 0.0017(11) 0.0086(11) -0.0020(10) 0.0010(9) 0.0016(10) N3 0.0059(12) 0.0017(11) 0.0086(11) -0.0020(10) 0.0010(9) 0.0016(10) C15 0.0141(19) 0.009(2) 0.0150(17) -0.0038(18) 0.0065(12) -0.0067(18) C18 0.013(2) 0.018(2) 0.0041(15) 0.0004(15) 0.0007(16) 0.001(2) Ag3 0.01029(16) 0.00970(14) 0.00555(14) 0.00680(14) -0.00119(12) -0.00147(15) Ag2 0.0224(2) 0.0235(2) 0.0193(2) -0.00026(19) 0.00150(18) 0.00133(19) Ag1 0.01210(13) 0.01343(12) 0.01179(13) -0.0069(2) 0.00578(10) 0.0016(2) Fe1 0.0083(3) 0.0058(2) 0.0049(2) -0.0029(2) 0.00280(19) 0.0023(2) N2 0.0089(9) 0.0107(8) 0.0064(10) -0.0010(8) 0.0049(8) 0.0023(8) N1 0.0089(9) 0.0107(8) 0.0064(10) -0.0010(8) 0.0049(8) 0.0023(8) N4 0.0083(18) 0.0138(16) 0.0151(16) 0.0014(13) 0.0001(14) -0.0054(14) C2 0.0156(13) 0.0132(12) 0.0075(15) 0.0075(13) 0.0000(12) -0.0030(11) C1 0.0108(8) 0.0115(7) 0.0072(8) 0.0023(7) -0.0012(7) 0.0034(6) C9 0.0117(12) 0.0171(12) 0.0046(14) 0.0003(13) 0.0038(11) -0.0026(11) C8 0.0108(8) 0.0115(7) 0.0072(8) 0.0023(7) -0.0012(7) 0.0034(6) C3 0.0154(16) 0.0183(16) 0.007(2) 0.0027(19) -0.0003(17) -0.0015(14) C4 0.0156(13) 0.0132(12) 0.0075(15) 0.0075(13) 0.0000(12) -0.0030(11) C6 0.0144(11) 0.0181(13) 0.0135(13) -0.0042(12) -0.0012(11) -0.0023(10) C5 0.0108(8) 0.0115(7) 0.0072(8) 0.0023(7) -0.0012(7) 0.0034(6) C10 0.0171(16) 0.0182(16) 0.005(2) 0.0006(19) 0.0020(18) -0.0024(14) C7 0.0153(14) 0.0146(10) 0.0237(16) 0.0036(12) -0.0023(13) -0.0014(10) N5 0.0142(15) 0.0117(17) 0.0155(16) -0.0069(14) 0.0041(11) -0.0070(14) C17 0.021(2) 0.021(3) 0.0206(18) -0.004(2) 0.0067(12) 0.006(2) C16 0.018(3) 0.014(2) 0.0162(15) 0.0008(14) 0.0067(17) 0.003(2) C12 0.0108(8) 0.0115(7) 0.0072(8) 0.0023(7) -0.0012(7) 0.0034(6) C11 0.0117(12) 0.0171(12) 0.0046(14) 0.0003(13) 0.0038(11) -0.0026(11) C13 0.0144(11) 0.0181(13) 0.0135(13) -0.0042(12) -0.0012(11) -0.0023(10) C14 0.0153(14) 0.0146(10) 0.0237(16) 0.0036(12) -0.0023(13) -0.0014(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N8 C20 1.18(5) . ? N8 Ag2 1.99(3) . ? C20 Ag3 2.13(4) . ? N7 C19 1.154(9) . ? N7 Ag3 2.108(5) . ? C19 Ag2 2.020(8) . ? N6 C18 1.245(6) . ? N6 Fe1 1.953(4) 3_454 ? N3 C15 1.217(7) . ? N3 Fe1 1.873(5) 4_564 ? C15 Ag1 1.938(6) . ? C18 Ag3 1.952(5) . ? Ag3 Ag2 3.0703(6) 2_574 ? Ag2 C16 2.140(6) . ? Ag2 Ag3 3.0703(6) 2_575 ? Ag2 Ag1 3.3751(7) 3_455 ? Ag1 C17 2.158(7) . ? Ag1 Ag2 3.3751(7) 3_545 ? Fe1 N3 1.873(5) 4_465 ? Fe1 N4 1.915(5) . ? Fe1 N6 1.953(4) 3_546 ? Fe1 N2 1.966(4) . ? Fe1 N5 1.998(5) . ? Fe1 N1 2.025(4) . ? N2 C12 1.222(7) . ? N2 C8 1.384(7) . ? N1 C1 1.317(7) . ? N1 C5 1.469(7) . ? N4 C16 1.084(7) . ? C2 C1 1.385(7) . ? C2 C3 1.389(8) . ? C2 C6 1.473(8) . ? C1 H1 0.9500 . ? C9 C8 1.366(8) . ? C9 C10 1.405(8) . ? C9 C13 1.556(8) . ? C8 H8 0.9500 . ? C3 C4 1.430(8) . ? C3 H3 0.9500 . ? C4 C5 1.432(7) . ? C4 C7 1.529(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C5 H5 0.9500 . ? C10 C11 1.344(8) . ? C10 H10 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? N5 C17 1.085(9) . ? C12 C11 1.331(7) . ? C12 H12 0.9500 . ? C11 C14 1.492(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 C20 N8 Ag2 167(3) . . ? N8 C20 Ag3 167(3) . . ? C19 N7 Ag3 172.7(6) . . ? N7 C19 Ag2 176.5(7) . . ? C18 N6 Fe1 166.9(4) . 3_454 ? C15 N3 Fe1 171.8(4) . 4_564 ? N3 C15 Ag1 169.3(4) . . ? N6 C18 Ag3 177.5(5) . . ? C18 Ag3 N7 169.9(2) . . ? C18 Ag3 C20 171.2(9) . . ? N7 Ag3 C20 5.0(11) . . ? C18 Ag3 Ag2 71.74(17) . 2_574 ? N7 Ag3 Ag2 114.15(16) . 2_574 ? C20 Ag3 Ag2 109.1(11) . 2_574 ? N8 Ag2 C19 5.6(10) . . ? N8 Ag2 C16 172.7(10) . . ? C19 Ag2 C16 178.3(3) . . ? N8 Ag2 Ag3 111.6(10) . 2_575 ? C19 Ag2 Ag3 109.9(2) . 2_575 ? C16 Ag2 Ag3 70.81(18) . 2_575 ? N8 Ag2 Ag1 86.6(10) . 3_455 ? C19 Ag2 Ag1 81.1(2) . 3_455 ? C16 Ag2 Ag1 100.53(16) . 3_455 ? Ag3 Ag2 Ag1 63.946(17) 2_575 3_455 ? C15 Ag1 C17 169.0(2) . . ? C15 Ag1 Ag2 68.87(15) . 3_545 ? C17 Ag1 Ag2 122.18(17) . 3_545 ? N3 Fe1 N4 96.3(2) 4_465 . ? N3 Fe1 N6 85.13(18) 4_465 3_546 ? N4 Fe1 N6 173.56(19) . 3_546 ? N3 Fe1 N2 92.04(19) 4_465 . ? N4 Fe1 N2 93.48(19) . . ? N6 Fe1 N2 92.76(17) 3_546 . ? N3 Fe1 N5 174.4(2) 4_465 . ? N4 Fe1 N5 85.7(2) . . ? N6 Fe1 N5 92.36(19) 3_546 . ? N2 Fe1 N5 93.0(2) . . ? N3 Fe1 N1 86.26(19) 4_465 . ? N4 Fe1 N1 86.97(19) . . ? N6 Fe1 N1 86.84(17) 3_546 . ? N2 Fe1 N1 178.3(2) . . ? N5 Fe1 N1 88.65(19) . . ? C12 N2 C8 118.4(5) . . ? C12 N2 Fe1 123.5(4) . . ? C8 N2 Fe1 117.9(3) . . ? C1 N1 C5 114.7(4) . . ? C1 N1 Fe1 126.0(4) . . ? C5 N1 Fe1 118.7(3) . . ? C16 N4 Fe1 171.7(5) . . ? C1 C2 C3 117.8(5) . . ? C1 C2 C6 122.1(5) . . ? C3 C2 C6 120.2(5) . . ? N1 C1 C2 128.8(5) . . ? N1 C1 H1 115.6 . . ? C2 C1 H1 115.6 . . ? C8 C9 C10 117.2(5) . . ? C8 C9 C13 119.8(5) . . ? C10 C9 C13 123.0(5) . . ? C9 C8 N2 118.8(5) . . ? C9 C8 H8 120.6 . . ? N2 C8 H8 120.6 . . ? C2 C3 C4 119.2(5) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.4(5) . . ? C3 C4 C7 127.4(5) . . ? C5 C4 C7 112.5(5) . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.4 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C5 N1 119.7(5) . . ? C4 C5 H5 120.2 . . ? N1 C5 H5 120.2 . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C4 C7 H7A 109.4 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C17 N5 Fe1 168.3(5) . . ? N5 C17 Ag1 175.4(6) . . ? N4 C16 Ag2 167.6(5) . . ? N2 C12 C11 128.5(5) . . ? N2 C12 H12 115.7 . . ? C11 C12 H12 115.7 . . ? C12 C11 C10 115.4(5) . . ? C12 C11 C14 126.6(5) . . ? C10 C11 C14 117.4(5) . . ? C9 C13 H13A 109.4 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.4 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 5.152 _refine_diff_density_min -5.678 _refine_diff_density_rms 0.387