# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global #==================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'Tong, Ming-Liang' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Shi, Jian-Xin' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; 'Chen, Xiao-Ming' ; School of Chemistry and Chemical Engineering Zhongshan University Guangzhou 510275 P. R. China ; _publ_contact_author_name 'Dr Ming-Liang Tong' _publ_contact_author_address ; School of Chemistry & Chemical Engineering Sun Yat-Sen University 135 Xingang West Road Guangzhou 510275 510275 CHINA ; _publ_contact_author_phone '86-20-84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_coeditor_name ? _publ_requested_journal 'New Journal of Chemistry' # 3. TITLE AND AUTHOR LIST _publ_section_title ; Photoluminescent Two-Dimensional Coordination Polymers Constructed with Octanuclear Silver(I) Clusters or Silver(I) Ions ; data_complex_1 _database_code_CSD 163960 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H70 Ag8 N10 O26 S4' _chemical_formula_weight 2338.46 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' '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 10.554(7) _cell_length_b 12.210(8) _cell_length_c 14.290(5) _cell_angle_alpha 82.97(1) _cell_angle_beta 80.82(1) _cell_angle_gamma 89.79(1) _cell_volume 1804.0(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 2.327 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details '\y-scans (North et al., 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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 7371 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 26.99 _reflns_number_total 7355 _reflns_number_gt 5122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V.5.0 (Sheldrick, 1997)' _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^)+(0.0569P)^2^+1.9451P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7355 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.45512(5) 0.82829(5) 0.26536(4) 0.04854(16) Uani 1 d . . . Ag2 Ag 0.44149(5) 0.86838(4) 0.48644(4) 0.04420(15) Uani 1 d . . . Ag3 Ag 0.76657(5) 1.02135(5) 0.36236(4) 0.05059(17) Uani 1 d . . . Ag4 Ag 0.77246(5) 0.92119(5) 0.15091(4) 0.04935(16) Uani 1 d . . . S1 S 0.50267(13) 1.08864(12) 0.28287(11) 0.0308(3) Uani 1 d . . . S2 S 0.71249(14) 0.76163(13) 0.37130(12) 0.0353(4) Uani 1 d . . . O1 O 0.4187(4) 1.0124(4) 0.2469(3) 0.0438(11) Uani 1 d . . . O2 O 0.4920(5) 1.0577(4) 0.3877(3) 0.0460(12) Uani 1 d . . . O3 O 0.6369(4) 1.0772(4) 0.2370(4) 0.0540(13) Uani 1 d . . . O4 O 0.4614(5) 1.2023(4) 0.2631(3) 0.0542(13) Uani 1 d . . . O5 O 0.6671(4) 0.8588(4) 0.4205(4) 0.0612(15) Uani 1 d . . . O6 O 0.8170(4) 0.7983(4) 0.2940(3) 0.0504(12) Uani 1 d . . . O7 O 0.6040(5) 0.7191(4) 0.3325(4) 0.0596(14) Uani 1 d . . . O8 O 0.7556(5) 0.6781(4) 0.4397(4) 0.0563(13) Uani 1 d . . . N1 N 0.3345(5) 0.7000(4) 0.2109(4) 0.0389(12) Uani 1 d . . . N2 N -0.0594(5) 1.0383(4) 0.1208(4) 0.0375(12) Uani 1 d . . . N3 N 0.2844(4) 0.7671(4) 0.4513(3) 0.0308(11) Uani 1 d . . . N4 N -0.0726(4) 1.1370(4) 0.3532(3) 0.0328(11) Uani 1 d . . . N5 N 0.6471(5) 0.8134(4) 0.0888(4) 0.0341(11) Uani 1 d . . . C1 C 0.3667(7) 0.5935(6) 0.2226(5) 0.0491(17) Uani 1 d . . . H1A H 0.4398 0.5743 0.2531 0.080 Uiso 1 d R . . C2 C 0.2996(8) 0.5112(6) 0.1916(6) 0.061(2) Uani 1 d . . . H2A H 0.3252 0.4358 0.2022 0.080 Uiso 1 d R . . C3 C 0.1956(8) 0.5382(7) 0.1480(7) 0.069(2) Uani 1 d . . . H3A H 0.1485 0.4829 0.1249 0.080 Uiso 1 d R . . C4 C 0.1610(7) 0.6478(6) 0.1362(6) 0.0536(19) Uani 1 d . . . H4A H 0.0888 0.6690 0.1052 0.080 Uiso 1 d R . . C5 C 0.2300(6) 0.7281(5) 0.1679(5) 0.0383(15) Uani 1 d . . . C6 C 0.1997(6) 0.8440(6) 0.1581(5) 0.0421(16) Uani 1 d . . . H6A H 0.2677 0.8945 0.1618 0.080 Uiso 1 d R . . C7 C 0.0877(6) 0.8894(5) 0.1440(4) 0.0390(15) Uani 1 d . . . H7A H 0.0191 0.8394 0.1403 0.080 Uiso 1 d R . . C8 C 0.0615(6) 1.0094(5) 0.1324(4) 0.0360(14) Uani 1 d . . . C9 C 0.1556(6) 1.0887(6) 0.1331(5) 0.0454(17) Uani 1 d . . . H9A H 0.2407 1.0671 0.1423 0.080 Uiso 1 d R . . C10 C 0.1249(7) 1.1998(6) 0.1179(5) 0.0506(18) Uani 1 d . . . H10A H 0.1882 1.2557 0.1189 0.080 Uiso 1 d R . . C11 C 0.0042(8) 1.2292(6) 0.1026(5) 0.0555(19) Uani 1 d . . . H11A H -0.0177 1.3053 0.0896 0.080 Uiso 1 d R . . C12 C -0.0865(7) 1.1469(6) 0.1059(5) 0.0466(17) Uani 1 d . . . H12A H -0.1724 1.1668 0.0974 0.080 Uiso 1 d R . . C13 C 0.2966(6) 0.6559(5) 0.4672(5) 0.0389(15) Uani 1 d . . . H13A H 0.3744 0.6275 0.4869 0.080 Uiso 1 d R . . C14 C 0.2029(6) 0.5818(5) 0.4552(5) 0.0457(17) Uani 1 d . . . H14A H 0.2130 0.5037 0.4702 0.080 Uiso 1 d R . . C15 C 0.0946(6) 0.6229(5) 0.4228(5) 0.0418(16) Uani 1 d . . . H15A H 0.0289 0.5738 0.4121 0.080 Uiso 1 d R . . C16 C 0.0791(5) 0.7363(5) 0.4052(4) 0.0333(13) Uani 1 d . . . H16A H 0.0035 0.7661 0.3829 0.080 Uiso 1 d R . . C17 C 0.1765(5) 0.8082(5) 0.4204(4) 0.0282(12) Uani 1 d . . . C18 C 0.1649(5) 0.9292(5) 0.4069(4) 0.0319(13) Uani 1 d . . . H18A H 0.2382 0.9730 0.4121 0.080 Uiso 1 d R . . C19 C 0.0595(5) 0.9821(5) 0.3882(4) 0.0313(13) Uani 1 d . . . H19A H -0.0140 0.9371 0.3859 0.080 Uiso 1 d R . . C20 C 0.0441(5) 1.1027(5) 0.3715(4) 0.0301(13) Uani 1 d . . . C21 C 0.1403(6) 1.1783(5) 0.3772(5) 0.0407(15) Uani 1 d . . . H21A H 0.2212 1.1525 0.3929 0.080 Uiso 1 d R . . C22 C 0.1190(7) 1.2907(6) 0.3596(5) 0.0483(17) Uani 1 d . . . H22A H 0.1838 1.3439 0.3639 0.080 Uiso 1 d R . . C23 C 0.0015(7) 1.3250(6) 0.3372(5) 0.0478(17) Uani 1 d . . . H23A H -0.0152 1.4019 0.3222 0.080 Uiso 1 d R . . C24 C -0.0924(6) 1.2466(5) 0.3355(4) 0.0384(15) Uani 1 d . . . H24A H -0.1747 1.2708 0.3213 0.080 Uiso 1 d R . . C25 C 0.6730(6) 0.7052(5) 0.0973(5) 0.0428(16) Uani 1 d . . . H25A H 0.7313 0.6778 0.1395 0.080 Uiso 1 d R . . C26 C 0.6192(7) 0.6311(6) 0.0466(5) 0.0483(17) Uani 1 d . . . H26A H 0.6408 0.5544 0.0527 0.080 Uiso 1 d R . . C27 C 0.5340(7) 0.6716(6) -0.0130(5) 0.0478(17) Uani 1 d . . . H27A H 0.4933 0.6233 -0.0478 0.080 Uiso 1 d R . . C28 C 0.5062(6) 0.7834(6) -0.0207(5) 0.0424(16) Uani 1 d . . . H28A H 0.4484 0.8133 -0.0623 0.080 Uiso 1 d R . . C29 C 0.5624(5) 0.8536(5) 0.0308(4) 0.0303(13) Uani 1 d . . . C30 C 0.5381(5) 0.9717(5) 0.0267(4) 0.0323(13) Uani 1 d . . . H30A H 0.5811 1.0126 0.0660 0.080 Uiso 1 d R . . O1W O 0.6740(6) 1.3608(5) 0.1658(5) 0.092(2) Uani 1 d . . . H1WB H 0.6812 1.2893 0.1633 0.100 Uiso 1 d R . . H1WA H 0.7549 1.3874 0.1580 0.100 Uiso 1 d R . . O2W O 0.4453(6) 1.3464(5) 0.4003(4) 0.0754(18) Uani 1 d . . . H2WA H 0.4405 1.2840 0.3733 0.100 Uiso 1 d R . . H2WB H 0.3823 1.3443 0.4659 0.100 Uiso 1 d R . . O3W O 0.3599(7) 1.5138(5) 0.6793(5) 0.100(2) Uani 1 d . . . H3WA H 0.2886 1.5613 0.7005 0.100 Uiso 1 d R . . H3WB H 0.3156 1.4487 0.6619 0.100 Uiso 1 d R . . O4W O -0.1152(10) 0.5710(10) 0.2540(9) 0.176(4) Uani 1 d . . . O5W O -0.0994(11) 0.4979(12) 0.0729(9) 0.203(5) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0453(3) 0.0551(4) 0.0483(3) -0.0107(3) -0.0137(2) -0.0023(2) Ag2 0.0334(3) 0.0487(3) 0.0549(3) -0.0118(3) -0.0162(2) -0.0044(2) Ag3 0.0328(3) 0.0497(3) 0.0733(4) -0.0131(3) -0.0164(3) -0.0044(2) Ag4 0.0427(3) 0.0481(3) 0.0620(4) -0.0026(3) -0.0257(3) -0.0058(2) S1 0.0310(7) 0.0333(8) 0.0292(8) -0.0038(6) -0.0079(6) -0.0013(6) S2 0.0303(7) 0.0357(9) 0.0394(9) 0.0037(7) -0.0099(6) -0.0011(6) O1 0.039(2) 0.051(3) 0.046(3) -0.015(2) -0.016(2) -0.008(2) O2 0.080(3) 0.040(3) 0.021(2) -0.0037(19) -0.018(2) -0.006(2) O3 0.032(2) 0.075(4) 0.058(3) -0.019(3) -0.008(2) -0.002(2) O4 0.072(3) 0.042(3) 0.048(3) -0.004(2) -0.011(3) 0.011(2) O5 0.044(3) 0.044(3) 0.092(4) -0.013(3) 0.005(3) -0.004(2) O6 0.032(2) 0.073(4) 0.041(3) 0.009(2) 0.000(2) -0.002(2) O7 0.049(3) 0.068(4) 0.066(4) -0.004(3) -0.024(3) -0.015(2) O8 0.053(3) 0.057(3) 0.055(3) 0.019(3) -0.016(2) 0.005(2) N1 0.040(3) 0.045(3) 0.032(3) -0.004(2) -0.008(2) -0.002(2) N2 0.036(3) 0.044(3) 0.031(3) 0.004(2) -0.008(2) -0.008(2) N3 0.025(2) 0.038(3) 0.032(3) -0.004(2) -0.009(2) -0.002(2) N4 0.033(3) 0.036(3) 0.029(3) -0.004(2) -0.004(2) 0.001(2) N5 0.038(3) 0.034(3) 0.031(3) -0.001(2) -0.011(2) 0.000(2) C1 0.052(4) 0.044(4) 0.050(4) -0.006(3) -0.003(3) 0.005(3) C2 0.067(5) 0.043(4) 0.068(6) -0.006(4) 0.001(4) 0.000(4) C3 0.077(6) 0.059(6) 0.075(6) -0.019(5) -0.019(5) -0.010(4) C4 0.046(4) 0.055(5) 0.068(5) -0.014(4) -0.028(4) -0.010(3) C5 0.036(3) 0.045(4) 0.035(4) -0.007(3) -0.005(3) -0.005(3) C6 0.038(3) 0.048(4) 0.042(4) -0.003(3) -0.011(3) -0.005(3) C7 0.033(3) 0.048(4) 0.037(4) -0.010(3) -0.007(3) -0.010(3) C8 0.035(3) 0.046(4) 0.028(3) -0.006(3) -0.006(3) -0.007(3) C9 0.043(4) 0.049(4) 0.045(4) -0.012(3) -0.004(3) -0.012(3) C10 0.057(4) 0.044(4) 0.052(5) -0.017(4) -0.003(4) -0.015(3) C11 0.069(5) 0.042(4) 0.051(5) -0.006(4) 0.001(4) -0.003(4) C12 0.049(4) 0.049(4) 0.042(4) 0.005(3) -0.014(3) -0.004(3) C13 0.036(3) 0.037(4) 0.044(4) -0.001(3) -0.009(3) 0.005(3) C14 0.049(4) 0.030(3) 0.056(5) 0.003(3) -0.010(3) 0.000(3) C15 0.043(4) 0.032(4) 0.054(4) -0.006(3) -0.017(3) -0.005(3) C16 0.029(3) 0.034(3) 0.038(4) -0.003(3) -0.011(3) -0.001(2) C17 0.026(3) 0.035(3) 0.023(3) -0.001(2) -0.004(2) -0.004(2) C18 0.030(3) 0.031(3) 0.033(3) -0.002(3) -0.005(2) -0.003(2) C19 0.030(3) 0.032(3) 0.032(3) -0.005(3) -0.007(2) -0.004(2) C20 0.034(3) 0.029(3) 0.029(3) -0.008(3) -0.007(2) -0.001(2) C21 0.037(3) 0.039(4) 0.046(4) -0.001(3) -0.009(3) -0.008(3) C22 0.063(4) 0.035(4) 0.046(4) 0.001(3) -0.009(3) -0.017(3) C23 0.071(5) 0.032(4) 0.042(4) -0.003(3) -0.015(4) -0.002(3) C24 0.050(4) 0.029(3) 0.037(4) -0.001(3) -0.013(3) 0.011(3) C25 0.042(4) 0.038(4) 0.049(4) -0.001(3) -0.013(3) 0.004(3) C26 0.053(4) 0.037(4) 0.053(5) -0.004(3) -0.005(3) -0.003(3) C27 0.061(4) 0.042(4) 0.040(4) -0.007(3) -0.003(3) -0.014(3) C28 0.048(4) 0.049(4) 0.034(4) -0.005(3) -0.015(3) -0.006(3) C29 0.028(3) 0.036(3) 0.028(3) -0.001(3) -0.008(2) -0.006(2) C30 0.028(3) 0.039(3) 0.030(3) -0.003(3) -0.008(2) -0.005(2) O1W 0.102(5) 0.081(5) 0.092(5) 0.000(4) -0.018(4) -0.030(4) O2W 0.092(4) 0.064(4) 0.067(4) -0.025(3) 0.010(3) -0.024(3) O3W 0.136(6) 0.070(4) 0.096(5) -0.007(4) -0.027(5) -0.041(4) O4W 0.136(9) 0.182(11) 0.210(12) -0.020(9) -0.035(8) 0.023(7) O5W 0.162(11) 0.244(14) 0.207(13) -0.044(11) -0.030(9) 0.047(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 Ag1 O1 2.269(5) . ? Ag1 N1 2.304(5) . ? Ag1 O7 2.307(5) . ? Ag1 Ag2 3.2364(13) . ? Ag2 N3 2.227(5) . ? Ag2 O2 2.312(4) 2_676 ? Ag2 O5 2.424(5) . ? Ag2 O2 2.567(5) . ? Ag2 Ag3 3.2372(13) 2_676 ? Ag3 N4 2.189(5) 1_655 ? Ag3 O5 2.251(5) . ? Ag3 O3 2.454(5) . ? Ag3 Ag2 3.2372(13) 2_676 ? Ag4 N5 2.223(5) . ? Ag4 N2 2.237(5) 1_655 ? Ag4 O6 2.491(5) . ? S1 O4 1.460(5) . ? S1 O3 1.477(5) . ? S1 O1 1.478(4) . ? S1 O2 1.486(4) . ? S2 O8 1.449(5) . ? S2 O6 1.460(5) . ? S2 O7 1.471(5) . ? S2 O5 1.491(5) . ? O2 Ag2 2.312(4) 2_676 ? O4 O2W 2.776(7) . ? O4 O1W 3.015(8) . ? N1 C1 1.340(8) . ? N1 C5 1.369(8) . ? N2 C8 1.352(8) . ? N2 C12 1.354(8) . ? N2 Ag4 2.237(5) 1_455 ? N3 C13 1.359(8) . ? N3 C17 1.359(7) . ? N4 C24 1.353(8) . ? N4 C20 1.355(7) . ? N4 Ag3 2.189(5) 1_455 ? N5 C25 1.344(8) . ? N5 C29 1.364(7) . ? C1 C2 1.387(10) . ? C2 C3 1.366(11) . ? C3 C4 1.383(11) . ? C4 C5 1.384(9) . ? C5 C6 1.445(9) . ? C6 C7 1.338(9) . ? C7 C8 1.485(9) . ? C8 C9 1.391(8) . ? C9 C10 1.392(10) . ? C10 C11 1.366(10) . ? C11 C12 1.381(10) . ? C13 C14 1.388(9) . ? C14 C15 1.372(9) . ? C15 C16 1.390(8) . ? C16 C17 1.413(8) . ? C17 C18 1.474(8) . ? C18 C19 1.332(8) . ? C19 C20 1.475(8) . ? C20 C21 1.393(8) . ? C21 C22 1.388(9) . ? C22 C23 1.381(10) . ? C23 C24 1.386(9) . ? C25 C26 1.399(9) . ? C26 C27 1.384(10) . ? C27 C28 1.389(10) . ? C28 C29 1.388(8) . ? C29 C30 1.459(8) . ? C30 C30 1.330(11) 2_675 ? O1W O5W 2.959(15) 1_665 ? O2W O8 2.846(7) 2_676 ? O3W O2W 2.691(9) 2_686 ? O3W O1W 2.819(10) 2_686 ? 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 O1 Ag1 N1 123.65(17) . . ? O1 Ag1 O7 134.31(16) . . ? N1 Ag1 O7 102.04(18) . . ? O1 Ag1 Ag2 82.28(11) . . ? N1 Ag1 Ag2 125.39(13) . . ? O7 Ag1 Ag2 70.70(14) . . ? N3 Ag2 O2 141.87(17) . 2_676 ? N3 Ag2 O5 125.43(18) . . ? O2 Ag2 O5 86.65(18) 2_676 . ? N3 Ag2 O2 117.58(16) . . ? O2 Ag2 O2 87.29(14) 2_676 . ? O5 Ag2 O2 76.20(16) . . ? N3 Ag2 Ag1 62.87(13) . . ? O2 Ag2 Ag1 155.18(12) 2_676 . ? O5 Ag2 Ag1 73.33(14) . . ? O2 Ag2 Ag1 73.99(10) . . ? N3 Ag2 Ag3 89.31(13) . 2_676 ? O2 Ag2 Ag3 60.36(13) 2_676 2_676 ? O5 Ag2 Ag3 145.18(13) . 2_676 ? O2 Ag2 Ag3 90.44(11) . 2_676 ? Ag1 Ag2 Ag3 134.09(3) . 2_676 ? N4 Ag3 O5 150.52(19) 1_655 . ? N4 Ag3 O3 110.76(18) 1_655 . ? O5 Ag3 O3 98.06(19) . . ? N4 Ag3 Ag2 99.17(13) 1_655 2_676 ? O5 Ag3 Ag2 86.86(13) . 2_676 ? O3 Ag3 Ag2 89.42(12) . 2_676 ? N5 Ag4 N2 145.72(19) . 1_655 ? N5 Ag4 O6 101.69(17) . . ? N2 Ag4 O6 102.59(17) 1_655 . ? O4 S1 O3 110.2(3) . . ? O4 S1 O1 110.2(3) . . ? O3 S1 O1 109.6(3) . . ? O4 S1 O2 109.6(3) . . ? O3 S1 O2 109.6(3) . . ? O1 S1 O2 107.7(3) . . ? O8 S2 O6 110.9(3) . . ? O8 S2 O7 110.3(3) . . ? O6 S2 O7 110.2(3) . . ? O8 S2 O5 109.1(3) . . ? O6 S2 O5 108.3(3) . . ? O7 S2 O5 107.9(3) . . ? S1 O1 Ag1 119.8(3) . . ? S1 O2 Ag2 136.4(3) . 2_676 ? S1 O2 Ag2 129.1(2) . . ? Ag2 O2 Ag2 92.71(14) 2_676 . ? S1 O3 Ag3 108.3(3) . . ? S1 O4 O2W 121.2(3) . . ? S1 O4 O1W 114.2(3) . . ? O2W O4 O1W 81.6(2) . . ? S2 O5 Ag3 116.5(3) . . ? S2 O5 Ag2 118.8(3) . . ? Ag3 O5 Ag2 115.8(2) . . ? S2 O6 Ag4 120.1(2) . . ? S2 O7 Ag1 124.4(3) . . ? C1 N1 C5 118.5(6) . . ? C1 N1 Ag1 118.9(4) . . ? C5 N1 Ag1 122.6(4) . . ? C8 N2 C12 118.6(5) . . ? C8 N2 Ag4 124.2(4) . 1_455 ? C12 N2 Ag4 116.2(4) . 1_455 ? C13 N3 C17 118.6(5) . . ? C13 N3 Ag2 116.2(4) . . ? C17 N3 Ag2 125.0(4) . . ? C24 N4 C20 118.7(5) . . ? C24 N4 Ag3 119.2(4) . 1_455 ? C20 N4 Ag3 121.9(4) . 1_455 ? C25 N5 C29 119.4(5) . . ? C25 N5 Ag4 116.5(4) . . ? C29 N5 Ag4 123.1(4) . . ? N1 C1 C2 122.6(7) . . ? C3 C2 C1 119.5(8) . . ? C2 C3 C4 118.4(7) . . ? C3 C4 C5 120.8(7) . . ? N1 C5 C4 120.2(6) . . ? N1 C5 C6 115.8(5) . . ? C4 C5 C6 124.0(6) . . ? C7 C6 C5 127.5(6) . . ? C6 C7 C8 125.7(6) . . ? N2 C8 C9 121.3(6) . . ? N2 C8 C7 116.5(5) . . ? C9 C8 C7 122.2(6) . . ? C8 C9 C10 118.9(6) . . ? C11 C10 C9 119.9(6) . . ? C10 C11 C12 118.6(7) . . ? N2 C12 C11 122.6(7) . . ? N3 C13 C14 123.2(6) . . ? C15 C14 C13 118.3(6) . . ? C14 C15 C16 120.1(6) . . ? C15 C16 C17 119.3(5) . . ? N3 C17 C16 120.5(5) . . ? N3 C17 C18 117.0(5) . . ? C16 C17 C18 122.4(5) . . ? C19 C18 C17 124.5(5) . . ? C18 C19 C20 126.6(5) . . ? N4 C20 C21 121.0(5) . . ? N4 C20 C19 115.7(5) . . ? C21 C20 C19 123.3(5) . . ? C22 C21 C20 119.9(6) . . ? C23 C22 C21 118.7(6) . . ? C22 C23 C24 119.1(6) . . ? N4 C24 C23 122.4(6) . . ? N5 C25 C26 122.7(6) . . ? C27 C26 C25 118.1(7) . . ? C26 C27 C28 119.0(6) . . ? C29 C28 C27 120.7(6) . . ? N5 C29 C28 120.0(6) . . ? N5 C29 C30 116.0(5) . . ? C28 C29 C30 124.0(5) . . ? C30 C30 C29 126.0(7) 2_675 . ? O5W O1W O4 174.2(4) 1_665 . ? O4 O2W O8 120.4(2) . 2_676 ? O2W O3W O1W 86.9(2) 2_686 2_686 ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.568 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.121 #===============================END data_complex_2 _database_code_CSD 163961 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 Ag N4 O2' _chemical_formula_weight 427.21 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.461(7) _cell_length_b 17.530(7) _cell_length_c 9.266(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.20(1) _cell_angle_gamma 90.00 _cell_volume 1768.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description polyhedral _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.158 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_T_max 0.641 _exptl_absorpt_process_details '\y-scans (North et al., 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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% none _diffrn_reflns_number 3821 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3583 _reflns_number_gt 2130 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-Plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-Plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL V.5.0 (Sheldrick, 1997)' _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^)+(0.0568P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3583 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1028 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.24441(4) 0.56661(2) 0.19077(5) 0.0580(2) Uani 1 d . . . N1 N 0.0754(4) 0.6302(2) 0.2427(5) 0.0492(11) Uani 1 d . . . N2 N 0.3893(4) 0.8303(3) 0.7411(5) 0.0533(12) Uani 1 d . . . N3 N 0.2363(4) 0.5498(3) -0.0717(5) 0.0556(12) Uani 1 d . . . N4 N 0.2745(7) 0.4128(3) 0.3223(8) 0.0877(19) Uani 1 d . . . O1 O 0.3527(5) 0.4641(4) 0.3562(6) 0.1026(18) Uani 1 d . . . O2 O 0.1789(6) 0.4326(3) 0.2296(7) 0.1049(17) Uani 1 d . . . C1 C -0.0365(5) 0.6173(3) 0.1433(6) 0.0592(15) Uani 1 d . . . H1A H -0.0443 0.5773 0.0702 0.080 Uiso 1 d R . . C2 C -0.1373(6) 0.6581(4) 0.1404(8) 0.076(2) Uani 1 d . . . H2A H -0.2156 0.6461 0.0681 0.080 Uiso 1 d R . . C3 C -0.1265(6) 0.7157(5) 0.2439(9) 0.094(2) Uani 1 d . . . H3A H -0.1968 0.7457 0.2430 0.080 Uiso 1 d R . . C4 C -0.0130(6) 0.7297(4) 0.3479(8) 0.078(2) Uani 1 d . . . H4A H -0.0031 0.7698 0.4213 0.080 Uiso 1 d R . . C5 C 0.0873(5) 0.6865(3) 0.3463(6) 0.0496(13) Uani 1 d . . . C6 C 0.2100(5) 0.6966(3) 0.4562(6) 0.0544(14) Uani 1 d . . . H6A H 0.2701 0.6581 0.4583 0.080 Uiso 1 d R . . C7 C 0.2467(5) 0.7533(3) 0.5539(6) 0.0532(14) Uani 1 d . . . H7A H 0.1873 0.7927 0.5486 0.080 Uiso 1 d R . . C8 C 0.3677(5) 0.7625(3) 0.6692(6) 0.0487(13) Uani 1 d . . . C9 C 0.4537(6) 0.7043(4) 0.7053(7) 0.0730(18) Uani 1 d . . . H9A H 0.4353 0.6564 0.6526 0.080 Uiso 1 d R . . C10 C 0.5648(6) 0.7159(5) 0.8172(8) 0.095(3) Uani 1 d . . . H10A H 0.6253 0.6760 0.8444 0.080 Uiso 1 d R . . C11 C 0.5876(6) 0.7843(4) 0.8906(8) 0.081(2) Uani 1 d . . . H11A H 0.6647 0.7943 0.9669 0.080 Uiso 1 d R . . C12 C 0.4977(5) 0.8397(4) 0.8488(6) 0.0633(16) Uani 1 d . . . H12A H 0.5133 0.8874 0.9021 0.080 Uiso 1 d R . . C13 C 0.1293(5) 0.5646(3) -0.1805(7) 0.0627(15) Uani 1 d . . . H13A H 0.0623 0.5842 -0.1502 0.080 Uiso 1 d R . . C14 C 0.1101(6) 0.5523(4) -0.3326(7) 0.0712(18) Uani 1 d . . . H14A H 0.0323 0.5633 -0.4068 0.080 Uiso 1 d R . . C15 C 0.2051(7) 0.5248(4) -0.3759(8) 0.0744(19) Uani 1 d . . . H15A H 0.1945 0.5150 -0.4811 0.080 Uiso 1 d R . . C16 C 0.3155(6) 0.5107(4) -0.2682(7) 0.0704(18) Uani 1 d . . . H16A H 0.3832 0.4917 -0.2977 0.080 Uiso 1 d R . . C17 C 0.3313(5) 0.5235(3) -0.1153(6) 0.0539(14) Uani 1 d . . . C18 C 0.4466(5) 0.5092(3) 0.0071(7) 0.0594(15) Uani 1 d . . . H18A H 0.4438 0.5130 0.1093 0.080 Uiso 1 d 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 0.0618(3) 0.0524(3) 0.0563(3) 0.0004(2) 0.0132(2) 0.0038(2) N1 0.046(3) 0.050(3) 0.050(3) -0.006(2) 0.013(2) -0.004(2) N2 0.046(3) 0.053(3) 0.051(3) -0.007(2) 0.001(2) -0.004(2) N3 0.053(3) 0.063(3) 0.050(3) -0.002(2) 0.014(2) 0.001(2) N4 0.110(6) 0.062(4) 0.091(5) 0.023(3) 0.033(5) 0.029(4) O1 0.083(4) 0.103(4) 0.103(4) 0.037(3) 0.002(3) 0.011(3) O2 0.104(4) 0.089(4) 0.100(4) 0.003(3) 0.001(3) -0.010(3) C1 0.053(4) 0.060(4) 0.057(4) 0.002(3) 0.005(3) -0.011(3) C2 0.046(4) 0.091(5) 0.075(5) 0.003(4) -0.004(3) -0.010(4) C3 0.049(4) 0.106(6) 0.116(6) -0.016(5) 0.008(4) 0.019(4) C4 0.052(4) 0.090(5) 0.087(5) -0.030(4) 0.012(4) 0.005(4) C5 0.045(3) 0.051(3) 0.050(3) -0.006(3) 0.011(3) -0.004(3) C6 0.048(3) 0.063(4) 0.051(3) -0.012(3) 0.014(3) 0.000(3) C7 0.048(3) 0.052(3) 0.054(3) -0.006(3) 0.008(3) 0.003(3) C8 0.048(3) 0.057(3) 0.039(3) -0.006(3) 0.012(3) 0.002(3) C9 0.066(4) 0.070(4) 0.069(4) -0.017(3) 0.000(3) 0.010(3) C10 0.068(4) 0.109(6) 0.084(5) -0.026(5) -0.013(4) 0.039(4) C11 0.052(4) 0.097(5) 0.072(4) -0.021(4) -0.011(3) 0.011(4) C12 0.059(4) 0.068(4) 0.055(4) -0.009(3) 0.006(3) -0.007(3) C13 0.059(4) 0.066(4) 0.058(4) -0.004(3) 0.011(3) 0.001(3) C14 0.060(4) 0.085(5) 0.060(4) -0.003(4) 0.006(3) -0.006(4) C15 0.083(5) 0.087(5) 0.049(4) -0.002(4) 0.015(4) 0.000(4) C16 0.076(5) 0.082(5) 0.056(4) -0.006(4) 0.026(4) 0.005(4) C17 0.056(4) 0.053(3) 0.049(4) 0.001(3) 0.011(3) 0.000(3) C18 0.062(4) 0.069(4) 0.048(3) -0.004(3) 0.019(3) 0.004(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 N2 2.400(5) 4_575 ? Ag1 N1 2.410(4) . ? Ag1 N3 2.423(5) . ? Ag1 O1 2.435(5) . ? Ag1 O2 2.526(5) . ? N1 C1 1.344(6) . ? N1 C5 1.354(6) . ? N2 C12 1.338(7) . ? N2 C8 1.347(6) . ? N2 Ag1 2.400(5) 4_576 ? N3 C13 1.347(7) . ? N3 C17 1.355(7) . ? N4 O2 1.213(8) . ? N4 O1 1.239(8) . ? C1 C2 1.352(8) . ? C2 C3 1.372(9) . ? C3 C4 1.377(9) . ? C4 C5 1.381(8) . ? C5 C6 1.467(7) . ? C6 C7 1.322(7) . ? C7 C8 1.471(7) . ? C8 C9 1.386(8) . ? C9 C10 1.384(8) . ? C10 C11 1.364(9) . ? C11 C12 1.379(8) . ? C13 C14 1.373(9) . ? C14 C15 1.360(9) . ? C15 C16 1.367(9) . ? C16 C17 1.389(8) . ? C17 C18 1.469(7) . ? C18 C18 1.311(10) 3_665 ? 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 99.39(15) 4_575 . ? N2 Ag1 N3 95.38(15) 4_575 . ? N1 Ag1 N3 118.38(15) . . ? N2 Ag1 O1 104.34(18) 4_575 . ? N1 Ag1 O1 119.96(18) . . ? N3 Ag1 O1 113.23(18) . . ? N2 Ag1 O2 153.03(17) 4_575 . ? N1 Ag1 O2 96.26(18) . . ? N3 Ag1 O2 96.32(17) . . ? O1 Ag1 O2 48.7(2) . . ? C1 N1 C5 118.1(5) . . ? C1 N1 Ag1 116.1(4) . . ? C5 N1 Ag1 124.8(3) . . ? C12 N2 C8 117.5(5) . . ? C12 N2 Ag1 118.5(4) . 4_576 ? C8 N2 Ag1 124.0(3) . 4_576 ? C13 N3 C17 118.1(5) . . ? C13 N3 Ag1 117.9(4) . . ? C17 N3 Ag1 123.9(4) . . ? O2 N4 O1 113.2(6) . . ? N4 O1 Ag1 100.9(4) . . ? N4 O2 Ag1 97.2(5) . . ? N1 C1 C2 123.5(6) . . ? C1 C2 C3 119.0(6) . . ? C2 C3 C4 118.7(6) . . ? C3 C4 C5 120.1(6) . . ? N1 C5 C4 120.6(5) . . ? N1 C5 C6 116.2(5) . . ? C4 C5 C6 123.2(5) . . ? C7 C6 C5 126.7(5) . . ? C6 C7 C8 127.3(5) . . ? N2 C8 C9 121.5(5) . . ? N2 C8 C7 116.3(5) . . ? C9 C8 C7 122.2(5) . . ? C10 C9 C8 119.4(6) . . ? C11 C10 C9 119.4(6) . . ? C10 C11 C12 118.0(6) . . ? N2 C12 C11 124.1(6) . . ? N3 C13 C14 123.7(6) . . ? C15 C14 C13 118.1(6) . . ? C14 C15 C16 119.5(6) . . ? C15 C16 C17 120.8(6) . . ? N3 C17 C16 119.8(5) . . ? N3 C17 C18 116.2(5) . . ? C16 C17 C18 124.0(5) . . ? C18 C18 C17 127.4(7) 3_665 . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.453 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.082 #_eof #End of Crystallographic Information File