Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author ; Stephen J. Loeb Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; _publ_contact_author_phone '+ 519 253-3000 ext 3529' _publ_contact_author_fax '+ 519 973-7098 ' _publ_contact_author_email loeb@uwindsor.ca _publ_requested_coeditor_name ? _publ_contact_letter ; This structure is one of two that are part of a study on the formation of metal ligand networks using the ligand 4,4'-bipyrimidine ; _publ_section_title ; Building coordination polymers with 4,4'-bipyrimidine. An infinite Ag(I) ladder and a heterometallic Co(II)-Ag(I)2 network ; loop_ _publ_author_name _publ_author_address S.J.Loeb ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; D.A.Beauchamp ; Department of Chemistry and Biochemistry University of Windsor Windsor, Ontario, Canada N9B 3P4 ; _publ_contact_author_name 'Stephen J. Loeb' data_[Ag(4,4'-bipyrimidine)Ag][OTf]2 _database_code_depnum_ccdc_archive 'CCDC 656381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H12 Ag3 F9 N8 O9 S3' _chemical_formula_weight 1087.16 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 7.8638(7) _cell_length_b 9.6992(9) _cell_length_c 11.2680(10) _cell_angle_alpha 84.012(2) _cell_angle_beta 88.758(2) _cell_angle_gamma 78.403(2) _cell_volume 837.30(13) _cell_formula_units_Z 1 _cell_measurement_temperature 566(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 2.032 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.824971 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 100 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6692 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2934 _reflns_number_gt 2451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.1241P)^2^+5.7035P] 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 2934 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.2020 _refine_ls_wR_factor_gt 0.1950 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.0000 0.0000 1.0000 0.0560(4) Uani 1 2 d S . . Ag2 Ag 0.30802(10) 0.11942(10) 1.47488(5) 0.0587(3) Uani 1 1 d . . . N1 N 0.2090(9) 0.0865(9) 0.8586(6) 0.0475(18) Uani 1 1 d . . . N2 N 0.3106(9) 0.1452(8) 0.6656(6) 0.0410(16) Uani 1 1 d . . . N3 N 0.2160(10) 0.0808(9) 1.1003(6) 0.0484(19) Uani 1 1 d . . . N4 N 0.3287(9) 0.1285(8) 1.2807(6) 0.0411(16) Uani 1 1 d . . . C1 C 0.2103(12) 0.0861(12) 0.7397(8) 0.051(2) Uani 1 1 d . . . H1A H 0.1327 0.0396 0.7071 0.061 Uiso 1 1 calc R . . C2 C 0.4216(14) 0.2140(11) 0.7115(8) 0.052(2) Uani 1 1 d . . . H2A H 0.4956 0.2561 0.6608 0.063 Uiso 1 1 calc R . . C3 C 0.4280(14) 0.2232(11) 0.8323(8) 0.052(2) Uani 1 1 d . . . H3A H 0.5020 0.2738 0.8638 0.063 Uiso 1 1 calc R . . C4 C 0.3190(9) 0.1537(8) 0.9060(6) 0.0321(16) Uani 1 1 d . . . C5 C 0.3255(9) 0.1475(9) 1.0386(7) 0.0339(16) Uani 1 1 d . . . C6 C 0.4459(12) 0.2044(11) 1.0955(7) 0.049(2) Uani 1 1 d . . . H6A H 0.5268 0.2479 1.0529 0.059 Uiso 1 1 calc R . . C7 C 0.4394(13) 0.1932(11) 1.2182(8) 0.050(2) Uani 1 1 d . . . H7A H 0.5162 0.2329 1.2589 0.060 Uiso 1 1 calc R . . C8 C 0.2242(12) 0.0753(12) 1.2171(7) 0.053(3) Uani 1 1 d . . . H8A H 0.1468 0.0281 1.2598 0.064 Uiso 1 1 calc R . . S1 S 0.1787(3) -0.2073(3) 1.5175(2) 0.0615(7) Uani 1 1 d . . . O1 O 0.3342(10) -0.1660(10) 1.5413(8) 0.077(2) Uani 1 1 d . . . O2 O 0.0326(15) -0.147(3) 1.5790(12) 0.195(9) Uani 1 1 d . . . O3 O 0.1498(15) -0.2060(12) 1.3905(8) 0.093(3) Uani 1 1 d . . . C9 C 0.219(6) -0.388(3) 1.5704(18) 0.188(16) Uani 1 1 d . . . F1 F 0.287(3) -0.4216(16) 1.6703(13) 0.220(10) Uani 1 1 d . . . F2 F 0.049(4) -0.412(3) 1.5749(19) 0.308(16) Uani 1 1 d . . . F3 F 0.309(5) -0.4722(17) 1.4964(19) 0.297(18) Uani 1 1 d . . . S2 S -0.1576(7) 0.3830(6) 0.9852(5) 0.0568(12) Uani 0.50 1 d P . . O4 O -0.1974(14) 0.2603(13) 0.9583(12) 0.047(3) Uani 0.50 1 d P . . O5 O 0.017(2) 0.3639(18) 1.0342(19) 0.085(5) Uani 0.50 1 d P . . O6 O -0.289(2) 0.4768(19) 1.0364(15) 0.080(5) Uani 0.50 1 d P . . C10 C -0.123(3) 0.461(2) 0.826(3) 0.069(7) Uani 0.50 1 d P . . F4 F -0.269(3) 0.4890(18) 0.7751(14) 0.118(7) Uani 0.50 1 d P . . F5 F -0.020(2) 0.3939(16) 0.7745(14) 0.089(5) Uani 0.50 1 d P . . F6 F -0.090(2) 0.5884(16) 0.8330(18) 0.098(5) Uani 0.50 1 d P . . 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 0.0456(6) 0.1011(9) 0.0343(5) -0.0088(5) 0.0014(4) -0.0448(6) Ag2 0.0542(5) 0.1107(7) 0.0180(4) -0.0072(3) 0.0020(3) -0.0328(4) N1 0.036(4) 0.090(6) 0.023(3) -0.007(3) 0.004(3) -0.029(4) N2 0.032(3) 0.072(5) 0.021(3) -0.006(3) -0.002(3) -0.014(3) N3 0.048(4) 0.082(5) 0.022(3) -0.002(3) -0.003(3) -0.030(4) N4 0.032(3) 0.069(5) 0.026(3) -0.006(3) -0.001(3) -0.017(3) C1 0.037(4) 0.096(7) 0.028(4) -0.007(4) 0.000(3) -0.031(5) C2 0.070(6) 0.071(6) 0.025(4) -0.001(4) 0.013(4) -0.038(5) C3 0.065(6) 0.070(6) 0.034(5) -0.010(4) 0.007(4) -0.040(5) C4 0.026(4) 0.049(4) 0.022(4) -0.002(3) 0.003(3) -0.009(3) C5 0.026(4) 0.046(4) 0.031(4) -0.004(3) -0.001(3) -0.010(3) C6 0.045(5) 0.083(7) 0.027(4) -0.003(4) 0.002(4) -0.034(5) C7 0.053(5) 0.083(7) 0.025(4) -0.004(4) -0.002(4) -0.036(5) C8 0.054(5) 0.096(7) 0.022(4) 0.003(4) 0.006(4) -0.049(5) S1 0.0429(13) 0.104(2) 0.0467(14) -0.0160(13) 0.0053(10) -0.0323(13) O1 0.051(4) 0.108(6) 0.078(6) 0.002(5) -0.007(4) -0.035(4) O2 0.070(7) 0.43(3) 0.095(9) -0.098(13) 0.024(6) -0.036(12) O3 0.119(8) 0.125(8) 0.046(5) -0.015(5) -0.004(5) -0.046(6) C9 0.38(5) 0.16(2) 0.068(11) 0.029(13) -0.047(19) -0.19(3) F1 0.40(3) 0.169(12) 0.122(10) 0.071(9) -0.112(14) -0.153(15) F2 0.43(3) 0.37(3) 0.22(2) 0.049(19) -0.01(2) -0.35(3) F3 0.55(5) 0.106(10) 0.187(18) -0.013(11) -0.13(2) 0.055(17) S2 0.050(3) 0.073(3) 0.050(3) -0.009(2) -0.003(2) -0.016(2) O4 0.023(5) 0.061(7) 0.066(8) -0.017(6) 0.006(5) -0.023(5) O5 0.070(11) 0.076(11) 0.111(15) -0.025(10) -0.032(10) -0.011(8) O6 0.074(11) 0.090(12) 0.063(10) 0.005(8) 0.012(8) 0.007(9) C10 0.048(12) 0.036(11) 0.12(2) 0.004(12) -0.020(13) 0.000(9) F4 0.18(2) 0.096(11) 0.060(9) -0.015(8) -0.038(11) 0.012(12) F5 0.121(13) 0.073(9) 0.072(9) -0.006(7) 0.043(9) -0.021(9) F6 0.082(10) 0.069(9) 0.135(15) 0.008(9) 0.029(10) -0.005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.362(7) 2_557 ? Ag1 N3 2.362(7) . ? Ag1 N1 2.471(7) 2_557 ? Ag1 N1 2.471(7) . ? Ag2 N4 2.185(7) . ? Ag2 N2 2.190(6) 1_556 ? N1 C4 1.333(10) . ? N1 C1 1.340(11) . ? N2 C1 1.304(11) . ? N2 C2 1.342(12) . ? N2 Ag2 2.190(6) 1_554 ? N3 C8 1.314(11) . ? N3 C5 1.321(11) . ? N4 C8 1.315(11) . ? N4 C7 1.323(11) . ? C2 C3 1.375(13) . ? C3 C4 1.401(12) . ? C4 C5 1.491(11) . ? C5 C6 1.386(11) . ? C6 C7 1.376(12) . ? S1 O2 1.386(12) . ? S1 O1 1.400(8) . ? S1 O3 1.452(9) . ? S1 C9 1.76(3) . ? C9 F1 1.24(2) . ? C9 F3 1.32(4) . ? C9 F2 1.40(4) . ? S2 O4 1.355(13) . ? S2 O6 1.389(17) . ? S2 O5 1.463(17) . ? S2 C10 1.91(3) . ? O5 F6 1.75(3) 2_567 ? C10 F5 1.12(3) . ? C10 F4 1.26(3) . ? C10 F6 1.32(3) . ? F6 O5 1.75(3) 2_567 ? 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 N3 Ag1 N3 180.0(1) 2_557 . ? N3 Ag1 N1 68.4(2) 2_557 2_557 ? N3 Ag1 N1 111.6(2) . 2_557 ? N3 Ag1 N1 111.6(2) 2_557 . ? N3 Ag1 N1 68.4(2) . . ? N1 Ag1 N1 180.0(2) 2_557 . ? N4 Ag2 N2 169.2(3) . 1_556 ? C4 N1 C1 117.5(7) . . ? C4 N1 Ag1 115.3(5) . . ? C1 N1 Ag1 126.8(6) . . ? C1 N2 C2 117.6(7) . . ? C1 N2 Ag2 120.5(6) . 1_554 ? C2 N2 Ag2 121.8(5) . 1_554 ? C8 N3 C5 116.7(7) . . ? C8 N3 Ag1 123.1(6) . . ? C5 N3 Ag1 119.9(5) . . ? C8 N4 C7 115.1(7) . . ? C8 N4 Ag2 121.6(5) . . ? C7 N4 Ag2 123.2(6) . . ? N2 C1 N1 125.8(8) . . ? N2 C2 C3 121.2(8) . . ? C2 C3 C4 117.5(8) . . ? N1 C4 C3 120.3(7) . . ? N1 C4 C5 117.8(7) . . ? C3 C4 C5 121.9(7) . . ? N3 C5 C6 121.1(7) . . ? N3 C5 C4 117.4(7) . . ? C6 C5 C4 121.5(7) . . ? C7 C6 C5 116.5(8) . . ? N4 C7 C6 122.8(8) . . ? N3 C8 N4 127.7(8) . . ? O2 S1 O1 116.9(8) . . ? O2 S1 O3 113.6(7) . . ? O1 S1 O3 112.3(6) . . ? O2 S1 C9 105.0(17) . . ? O1 S1 C9 103.3(12) . . ? O3 S1 C9 103.9(8) . . ? F1 C9 F3 108(4) . . ? F1 C9 F2 109(2) . . ? F3 C9 F2 108(2) . . ? F1 C9 S1 116.8(16) . . ? F3 C9 S1 114.3(17) . . ? F2 C9 S1 100(3) . . ? O4 S2 O6 116.6(10) . . ? O4 S2 O5 112.9(9) . . ? O6 S2 O5 117.3(12) . . ? O4 S2 C10 97.7(10) . . ? O6 S2 C10 107.8(10) . . ? O5 S2 C10 100.9(11) . . ? S2 O5 F6 131.0(14) . 2_567 ? F5 C10 F4 113(3) . . ? F5 C10 F6 112(2) . . ? F4 C10 F6 102.6(18) . . ? F5 C10 S2 114.5(16) . . ? F4 C10 S2 106.8(19) . . ? F6 C10 S2 107(2) . . ? C10 F6 O5 121.7(18) . 2_567 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.043 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.183 # Attachment 'CCDC 656382 revised Sept-7.CIF' data_dab55r _database_code_depnum_ccdc_archive 'CCDC 656382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H27 Ag2 Cl4 Co N13 O19' _chemical_formula_weight 1242.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 15.001(7) _cell_length_b 14.016(7) _cell_length_c 20.654(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4342(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 1.606 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.603937 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 100 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23176 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3822 _reflns_number_gt 3742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.0695P)^2^+69.9138P] 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 SHELXL _refine_ls_extinction_coef 0.0002(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3822 _refine_ls_number_parameters 370 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.1037 _refine_ls_wR_factor_ref 0.2468 _refine_ls_wR_factor_gt 0.2461 _refine_ls_goodness_of_fit_ref 1.299 _refine_ls_restrained_S_all 1.300 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.22221(13) -0.2500 0.5000 0.0318(5) Uani 1 2 d SD . . Ag1 Ag -0.43745(8) -0.15753(9) 0.7500 0.0400(4) Uani 1 2 d S . . Ag2 Ag -0.13479(8) -0.02679(10) 0.2500 0.0400(4) Uani 1 2 d S . . N1 N -0.3125(6) -0.1624(6) 0.5538(4) 0.0334(19) Uani 1 1 d . A . N2 N -0.3945(6) -0.1196(7) 0.6474(5) 0.040(2) Uani 1 1 d . A . N3 N -0.2020(6) -0.0356(6) 0.3482(4) 0.0335(19) Uani 1 1 d . A . N4 N -0.2366(6) -0.1295(6) 0.4401(4) 0.0294(18) Uani 1 1 d . A . C1 C -0.3459(8) -0.1798(8) 0.6115(5) 0.039(3) Uani 1 1 d . . . H1A H -0.3344 -0.2409 0.6295 0.047 Uiso 1 1 calc R A . C2 C -0.4128(10) -0.0356(9) 0.6205(6) 0.053(3) Uani 1 1 d . . . H2A H -0.4478 0.0090 0.6439 0.064 Uiso 1 1 calc R A . C3 C -0.3820(11) -0.0109(9) 0.5585(7) 0.060(4) Uani 1 1 d . A . H3A H -0.3964 0.0487 0.5393 0.073 Uiso 1 1 calc R . . C4 C -0.3297(8) -0.0771(7) 0.5266(6) 0.039(3) Uani 1 1 d . . . C5 C -0.2900(8) -0.0592(7) 0.4631(5) 0.034(2) Uani 1 1 d . A . C6 C -0.2990(8) 0.0245(8) 0.4290(6) 0.043(3) Uani 1 1 d . . . H6A H -0.3351 0.0750 0.4450 0.051 Uiso 1 1 calc R A . C7 C -0.2549(8) 0.0332(8) 0.3718(6) 0.040(3) Uani 1 1 d . A . H7A H -0.2618 0.0904 0.3475 0.048 Uiso 1 1 calc R . . C8 C -0.1964(7) -0.1144(8) 0.3840(5) 0.036(2) Uani 1 1 d . . . H8A H -0.1601 -0.1645 0.3678 0.043 Uiso 1 1 calc R A . Cl1 Cl -0.1713(3) -0.3032(3) 0.2500 0.0511(11) Uani 1 2 d S . . O1 O -0.2530(11) -0.2514(12) 0.2500 0.082(5) Uani 1 2 d S . . O2 O -0.1675(9) -0.3606(9) 0.1938(6) 0.092(4) Uani 1 1 d . . . O3 O -0.1000(12) -0.2378(13) 0.2500 0.105(7) Uani 1 2 d S . . Cl2 Cl -0.4170(2) -0.4359(3) 0.7500 0.0334(8) Uani 1 2 d S . . O4 O -0.4014(5) -0.3806(6) 0.8066(4) 0.049(2) Uani 1 1 d . . . O5 O -0.5088(7) -0.4652(8) 0.7500 0.044(3) Uani 1 2 d S . . O6 O -0.3617(9) -0.5193(9) 0.7500 0.053(3) Uani 1 2 d S . . Cl3 Cl 0.5369(3) 0.2500 0.5000 0.0612(13) Uani 1 2 d SD . . O7A O 0.596(3) 0.215(2) 0.4575(10) 0.39(3) Uani 1 1 d D . . O8A O 0.4863(10) 0.1869(11) 0.5407(12) 0.176(10) Uani 1 1 d D . . Cl4 Cl -0.0467(7) 0.0466(10) 0.5076(5) 0.114(5) Uani 0.50 1 d PD . . O11 O 0.0343(11) 0.021(2) 0.5437(9) 0.250(18) Uani 1 1 d D . . O10 O -0.1317(14) 0.032(2) 0.5417(12) 0.20(3) Uani 0.50 1 d PD . . O9 O -0.038(2) 0.1483(17) 0.501(3) 0.20(2) Uani 0.50 1 d PD . . N1S N -0.1107(18) -0.200(3) 0.5545(18) 0.031(6) Uani 0.50 1 d PDU A -1 C1S C -0.049(2) -0.187(3) 0.5832(19) 0.100(13) Uani 0.50 1 d PD A -1 C2S C 0.033(2) -0.178(4) 0.626(2) 0.17(3) Uani 0.50 1 d PD A -1 H2SA H 0.0714 -0.1264 0.6098 0.249 Uiso 0.50 1 calc PR A -1 H2SB H 0.0665 -0.2379 0.6260 0.249 Uiso 0.50 1 calc PR A -1 H2SC H 0.0147 -0.1628 0.6706 0.249 Uiso 0.50 1 calc PR A -1 O1W O -0.1340(19) -0.183(3) 0.558(2) 0.071(14) Uani 0.50 1 d PD A -2 H1WA H -0.0821 -0.2030 0.5490 0.106 Uiso 0.50 1 d PR A -2 H1WB H -0.1463 -0.1951 0.5971 0.106 Uiso 0.50 1 d PR A -2 O2W O -0.1336(17) 0.1630(14) 0.2500 0.184(16) Uani 1 2 d S . . H2WA H -0.1096 0.1827 0.2152 0.277 Uiso 1 1 d R . . N5 N -0.5672(8) -0.2441(10) 0.7500 0.040(3) Uani 1 2 d S . . C9 C -0.6067(8) -0.2700(9) 0.8044(6) 0.047(3) Uani 1 1 d . . . H9A H -0.5747 -0.2539 0.8431 0.056 Uiso 1 1 d R B . C10 C -0.690(3) -0.323(5) 0.813(2) 0.028(10) Uani 0.50 1 d PU B -1 H10A H -0.7107 -0.3433 0.8548 0.033 Uiso 0.50 1 d PR B -1 N6 N -0.681(4) -0.319(4) 0.798(2) 0.051(15) Uani 0.50 1 d P B -2 C11 C -0.7232(13) -0.3432(13) 0.7500 0.048(4) Uani 1 2 d S . . C12 C -0.8126(11) -0.3892(12) 0.7500 0.048(4) Uani 1 2 d S . . N7 N -0.849(3) -0.400(4) 0.808(2) 0.10(2) Uani 0.50 1 d P . -1 C13 C -0.857(3) -0.413(3) 0.805(2) 0.058(16) Uani 0.50 1 d PU . -2 H13A H -0.8219 -0.4192 0.8441 0.070 Uiso 0.50 1 d PR . -2 C14 C -0.9375(9) -0.4410(14) 0.8047(8) 0.072(5) Uani 1 1 d . . . H14A H -0.9736 -0.4393 0.8431 0.086 Uiso 1 1 d R . . N8 N -0.9823(9) -0.4560(10) 0.7500 0.054(4) Uani 1 2 d S . . O3W O -0.7825(11) -0.3278(14) 0.8869(7) 0.052(5) Uani 0.50 1 d P . . 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 Co1 0.0374(11) 0.0248(10) 0.0331(11) -0.0015(8) 0.000 0.000 Ag1 0.0453(7) 0.0479(8) 0.0267(6) 0.000 0.000 -0.0100(6) Ag2 0.0389(7) 0.0520(8) 0.0291(6) 0.000 0.000 0.0034(5) N1 0.050(5) 0.025(4) 0.026(4) -0.005(3) 0.006(4) -0.003(4) N2 0.050(5) 0.037(5) 0.034(5) -0.001(4) 0.006(4) -0.003(4) N3 0.038(5) 0.034(5) 0.029(4) 0.001(4) 0.001(4) 0.001(4) N4 0.043(5) 0.026(4) 0.020(4) -0.001(3) 0.004(4) -0.002(4) C1 0.061(7) 0.030(5) 0.028(5) 0.001(4) 0.003(5) -0.004(5) C2 0.082(9) 0.037(6) 0.040(7) 0.000(5) 0.022(6) 0.012(6) C3 0.098(11) 0.027(6) 0.057(8) 0.003(6) 0.028(8) 0.012(7) C4 0.056(7) 0.024(5) 0.039(6) -0.005(5) 0.012(5) 0.001(5) C5 0.054(6) 0.022(5) 0.027(5) -0.004(4) 0.005(5) -0.010(5) C6 0.054(7) 0.039(6) 0.036(6) 0.005(5) 0.010(5) 0.010(5) C7 0.051(6) 0.034(6) 0.036(6) 0.006(5) -0.004(5) -0.001(5) C8 0.041(6) 0.033(5) 0.033(6) -0.005(5) -0.002(5) -0.002(5) Cl1 0.057(3) 0.046(2) 0.050(2) 0.000 0.000 0.014(2) O1 0.079(10) 0.085(11) 0.081(11) 0.000 0.000 0.043(9) O2 0.105(9) 0.091(9) 0.079(8) -0.030(7) 0.001(7) 0.025(7) O3 0.073(11) 0.075(12) 0.17(2) 0.000 0.000 -0.008(10) Cl2 0.0366(19) 0.0331(18) 0.0306(18) 0.000 0.000 -0.0056(15) O4 0.043(4) 0.053(5) 0.050(5) -0.016(4) -0.009(4) -0.006(4) O5 0.034(6) 0.056(7) 0.041(6) 0.000 0.000 -0.023(5) O6 0.060(8) 0.046(7) 0.053(7) 0.000 0.000 0.007(6) Cl3 0.058(3) 0.042(2) 0.083(3) -0.017(2) 0.000 0.000 O7A 0.72(7) 0.35(4) 0.091(14) 0.051(19) 0.10(3) 0.44(5) O8A 0.106(11) 0.085(10) 0.34(3) 0.117(15) -0.055(15) -0.030(9) Cl4 0.086(6) 0.189(13) 0.069(6) -0.008(7) -0.009(5) -0.078(8) O11 0.144(18) 0.51(5) 0.094(13) -0.09(2) 0.022(12) -0.14(3) O10 0.25(5) 0.12(3) 0.22(4) -0.12(3) -0.21(4) 0.09(3) O9 0.14(3) 0.16(4) 0.29(6) 0.03(4) 0.00(4) -0.12(3) N1S 0.005(12) 0.047(14) 0.040(13) -0.002(10) -0.008(9) -0.005(11) C1S 0.13(4) 0.07(2) 0.10(3) -0.02(2) 0.02(3) 0.00(2) C2S 0.08(3) 0.23(6) 0.19(6) -0.13(5) 0.04(3) -0.10(4) O1W 0.030(17) 0.08(3) 0.10(2) -0.014(16) -0.015(16) -0.011(16) O2W 0.14(2) 0.044(10) 0.37(5) 0.000 0.000 0.029(12) N5 0.028(6) 0.040(7) 0.051(8) 0.000 0.000 -0.002(6) C9 0.036(6) 0.054(7) 0.050(7) 0.003(6) -0.001(6) -0.003(6) C10 0.017(13) 0.06(2) 0.002(12) 0.007(12) 0.002(12) -0.012(12) N6 0.07(2) 0.034(15) 0.05(3) 0.016(17) 0.030(17) 0.000(14) C11 0.049(10) 0.044(10) 0.051(13) 0.000 0.000 -0.008(8) C12 0.031(8) 0.037(9) 0.077(13) 0.000 0.000 0.003(7) N7 0.03(2) 0.18(5) 0.08(3) -0.01(3) 0.015(18) -0.01(2) C13 0.04(2) 0.059(19) 0.07(3) 0.06(2) -0.047(19) -0.041(17) C14 0.042(7) 0.108(13) 0.066(10) 0.014(9) -0.012(7) -0.010(8) N8 0.036(8) 0.028(7) 0.097(13) 0.000 0.000 0.003(6) O3W 0.045(9) 0.087(13) 0.026(8) 0.004(8) -0.009(7) -0.019(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1W 2.017(17) 4_546 ? Co1 O1W 2.017(17) . ? Co1 N4 2.105(8) . ? Co1 N4 2.105(8) 4_546 ? Co1 N1S 2.135(16) . ? Co1 N1S 2.135(16) 4_546 ? Co1 N1 2.139(9) 4_546 ? Co1 N1 2.139(9) . ? Ag1 N2 2.278(9) . ? Ag1 N2 2.278(9) 6_557 ? Ag1 N5 2.293(13) . ? Ag2 N3 2.269(9) 6_556 ? Ag2 N3 2.269(9) . ? Ag2 N8 2.299(14) 7_655 ? N1 C1 1.316(14) . ? N1 C4 1.346(14) . ? N2 C2 1.330(16) . ? N2 C1 1.338(15) . ? N3 C8 1.332(14) . ? N3 C7 1.340(14) . ? N4 C8 1.323(13) . ? N4 C5 1.356(13) . ? C2 C3 1.405(18) . ? C3 C4 1.382(16) . ? C4 C5 1.461(15) . ? C5 C6 1.375(15) . ? C6 C7 1.360(16) . ? Cl1 O2 1.413(12) . ? Cl1 O2 1.413(12) 6_556 ? Cl1 O3 1.409(18) . ? Cl1 O1 1.424(15) . ? Cl2 O4 1.422(8) 6_557 ? Cl2 O4 1.422(8) . ? Cl2 O6 1.434(13) . ? Cl2 O5 1.437(11) . ? Cl3 O7A 1.337(15) . ? Cl3 O7A 1.337(15) 4_556 ? Cl3 O8A 1.437(13) 4_556 ? Cl3 O8A 1.437(13) . ? Cl4 O11 1.43(3) 5_556 ? Cl4 O9 1.436(19) . ? Cl4 O11 1.471(17) . ? Cl4 O10 1.47(2) . ? Cl4 Cl4 1.94(3) 5_556 ? O11 Cl4 1.43(3) 5_556 ? N1S C1S 1.116(18) . ? C1S C2S 1.525(18) . ? N5 C9 1.321(14) . ? N5 C9 1.321(14) 6_557 ? C9 N6 1.31(6) . ? C9 C10 1.46(5) . ? C10 C11 1.43(4) . ? N6 C11 1.23(6) . ? C11 N6 1.23(6) 6_557 ? C11 C10 1.43(4) 6_557 ? C11 C12 1.49(2) . ? C12 N7 1.33(5) 6_557 ? C12 N7 1.33(5) . ? C12 C13 1.36(5) 6_557 ? C12 C13 1.36(5) . ? N7 C14 1.45(5) . ? C13 C14 1.27(5) . ? C14 N8 1.331(17) . ? N8 C14 1.331(17) 6_557 ? N8 Ag2 2.299(14) 7_456 ? 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 O1W Co1 O1W 98(2) 4_546 . ? O1W Co1 N4 95.5(16) 4_546 . ? O1W Co1 N4 92.3(15) . . ? O1W Co1 N4 92.3(15) 4_546 4_546 ? O1W Co1 N4 95.5(16) . 4_546 ? N4 Co1 N4 168.2(5) . 4_546 ? O1W Co1 N1S 87.2(11) 4_546 . ? O1W Co1 N1S 11.5(17) . . ? N4 Co1 N1S 97.3(12) . . ? N4 Co1 N1S 91.9(12) 4_546 . ? O1W Co1 N1S 11.5(17) 4_546 4_546 ? O1W Co1 N1S 87.2(11) . 4_546 ? N4 Co1 N1S 91.9(13) . 4_546 ? N4 Co1 N1S 97.3(12) 4_546 4_546 ? N1S Co1 N1S 77(2) . 4_546 ? O1W Co1 N1 80.7(11) 4_546 4_546 ? O1W Co1 N1 172.5(15) . 4_546 ? N4 Co1 N1 95.2(3) . 4_546 ? N4 Co1 N1 77.3(3) 4_546 4_546 ? N1S Co1 N1 163.4(11) . 4_546 ? N1S Co1 N1 92.0(10) 4_546 4_546 ? O1W Co1 N1 172.5(15) 4_546 . ? O1W Co1 N1 80.7(11) . . ? N4 Co1 N1 77.3(3) . . ? N4 Co1 N1 95.2(3) 4_546 . ? N1S Co1 N1 92.0(10) . . ? N1S Co1 N1 163.4(11) 4_546 . ? N1 Co1 N1 101.4(5) 4_546 . ? N2 Ag1 N2 137.0(5) . 6_557 ? N2 Ag1 N5 111.3(2) . . ? N2 Ag1 N5 111.3(2) 6_557 . ? N3 Ag2 N3 126.8(4) 6_556 . ? N3 Ag2 N8 115.9(2) 6_556 7_655 ? N3 Ag2 N8 115.9(2) . 7_655 ? C1 N1 C4 118.0(9) . . ? C1 N1 Co1 127.3(8) . . ? C4 N1 Co1 114.4(7) . . ? C2 N2 C1 116.0(10) . . ? C2 N2 Ag1 122.5(8) . . ? C1 N2 Ag1 121.5(7) . . ? C8 N3 C7 115.6(9) . . ? C8 N3 Ag2 120.9(7) . . ? C7 N3 Ag2 123.2(7) . . ? C8 N4 C5 117.4(9) . . ? C8 N4 Co1 126.6(7) . . ? C5 N4 Co1 116.0(6) . . ? N1 C1 N2 126.3(10) . . ? N2 C2 C3 122.1(11) . . ? C4 C3 C2 117.1(11) . . ? N1 C4 C3 120.4(10) . . ? N1 C4 C5 116.7(9) . . ? C3 C4 C5 122.9(10) . . ? N4 C5 C6 119.9(9) . . ? N4 C5 C4 115.4(9) . . ? C6 C5 C4 124.5(10) . . ? C7 C6 C5 118.3(11) . . ? N3 C7 C6 122.6(10) . . ? N4 C8 N3 126.1(10) . . ? O2 Cl1 O2 110.5(12) . 6_556 ? O2 Cl1 O3 109.9(7) . . ? O2 Cl1 O3 109.9(7) 6_556 . ? O2 Cl1 O1 108.9(7) . . ? O2 Cl1 O1 108.9(7) 6_556 . ? O3 Cl1 O1 108.7(11) . . ? O4 Cl2 O4 110.6(8) 6_557 . ? O4 Cl2 O6 110.4(5) 6_557 . ? O4 Cl2 O6 110.4(5) . . ? O4 Cl2 O5 108.3(4) 6_557 . ? O4 Cl2 O5 108.2(4) . . ? O6 Cl2 O5 108.8(8) . . ? O7A Cl3 O7A 97(4) . 4_556 ? O7A Cl3 O8A 100.9(13) . 4_556 ? O7A Cl3 O8A 120.5(18) 4_556 4_556 ? O7A Cl3 O8A 120.5(18) . . ? O7A Cl3 O8A 100.9(13) 4_556 . ? O8A Cl3 O8A 116.2(13) 4_556 . ? O11 Cl4 O9 125(3) 5_556 . ? O11 Cl4 O11 96.0(14) 5_556 . ? O9 Cl4 O11 103(2) . . ? O11 Cl4 O10 111.9(14) 5_556 . ? O9 Cl4 O10 105(2) . . ? O11 Cl4 O10 115.9(15) . . ? O11 Cl4 Cl4 48.9(11) 5_556 5_556 ? O9 Cl4 Cl4 126.1(17) . 5_556 ? O11 Cl4 Cl4 47.1(11) . 5_556 ? O10 Cl4 Cl4 127.3(17) . 5_556 ? Cl4 O11 Cl4 84.0(14) 5_556 . ? C1S N1S Co1 170(4) . . ? N1S C1S C2S 175(5) . . ? C9 N5 C9 116.4(14) . 6_557 ? C9 N5 Ag1 121.8(7) . . ? C9 N5 Ag1 121.8(7) 6_557 . ? N5 C9 N6 116(2) . . ? N5 C9 C10 129(2) . . ? N6 C9 C10 13(3) . . ? C11 C10 C9 107(3) . . ? C11 N6 C9 132(4) . . ? N6 C11 N6 108(5) 6_557 . ? N6 C11 C10 12(4) 6_557 6_557 ? N6 C11 C10 120(2) . 6_557 ? N6 C11 C10 120(2) 6_557 . ? N6 C11 C10 12(4) . . ? C10 C11 C10 132(4) 6_557 . ? N6 C11 C12 126(2) 6_557 . ? N6 C11 C12 126(2) . . ? C10 C11 C12 114(2) 6_557 . ? C10 C11 C12 114(2) . . ? N7 C12 N7 129(4) 6_557 . ? N7 C12 C13 9(4) 6_557 6_557 ? N7 C12 C13 122(2) . 6_557 ? N7 C12 C13 122(2) 6_557 . ? N7 C12 C13 9(4) . . ? C13 C12 C13 114(4) 6_557 . ? N7 C12 C11 115(2) 6_557 . ? N7 C12 C11 115(2) . . ? C13 C12 C11 122.9(19) 6_557 . ? C13 C12 C11 122.9(19) . . ? C12 N7 C14 112(4) . . ? C14 C13 C12 122(3) . . ? C13 C14 N8 123(3) . . ? C13 C14 N7 6(5) . . ? N8 C14 N7 125(2) . . ? C14 N8 C14 116.1(17) . 6_557 ? C14 N8 Ag2 121.3(8) . 7_456 ? C14 N8 Ag2 121.3(8) 6_557 7_456 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.869 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.180