# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Bao Li' _publ_contact_author_email libao@mail.hust.edu.cn loop_ _publ_author_name 'Wen-Jing Yu' 'Fan Yu' 'Tao-Tao Ding' 'Bao Li' 'Tian-Le Zhang' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 875528' #TrackingRef '- p.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H56 Ag3 N11 O21' _chemical_formula_weight 1470.66 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 'C 2/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 25.907(3) _cell_length_b 11.9344(12) _cell_length_c 23.796(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.356(2) _cell_angle_gamma 90.00 _cell_volume 6702.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8328 _exptl_absorpt_correction_T_max 0.9110 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Gemini S Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6336 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.75 _reflns_number_total 6336 _reflns_number_gt 4359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6336 _refine_ls_number_parameters 341 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1632 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.457405(18) -0.31069(4) 0.583754(19) 0.0661(2) Uani 1 1 d . . . Ag2 Ag 0.2500 0.7500 0.5000 0.0732(2) Uani 1 2 d S . . O2 O 0.28485(13) 0.3271(2) 0.36579(14) 0.0431(7) Uani 1 1 d . . . O4 O 0.16731(13) 0.0922(3) 0.26303(14) 0.0454(8) Uani 1 1 d . . . O1 O 0.30511(14) -0.0117(2) 0.35630(13) 0.0467(8) Uani 1 1 d . . . O3 O 0.29819(13) 0.2513(2) 0.23992(15) 0.0467(8) Uani 1 1 d . . . C9 C 0.2734(2) 0.4180(3) 0.3921(2) 0.0415(10) Uani 1 1 d . . . C21 C 0.12310(18) 0.0329(4) 0.22176(19) 0.0401(10) Uani 1 1 d . . . C6 C 0.2822(2) 0.0915(4) 0.3663(2) 0.0420(10) Uani 1 1 d . . . H6A H 0.3107 0.1325 0.4000 0.050 Uiso 1 1 calc R . . H6B H 0.2503 0.0772 0.3765 0.050 Uiso 1 1 calc R . . C24 C 0.21771(17) 0.0967(4) 0.25292(18) 0.0378(9) Uani 1 1 d . . . H24A H 0.2104 0.1353 0.2145 0.045 Uiso 1 1 calc R . . H24B H 0.2305 0.0214 0.2501 0.045 Uiso 1 1 calc R . . C22 C 0.1243(2) -0.0266(4) 0.1730(2) 0.0453(11) Uani 1 1 d . . . H22 H 0.1563 -0.0250 0.1647 0.054 Uiso 1 1 calc R . . C18 C 0.3147(2) 0.1753(4) 0.2921(2) 0.0417(10) Uani 1 1 d . . . H18A H 0.3459 0.2066 0.3274 0.050 Uiso 1 1 calc R . . H18B H 0.3266 0.1040 0.2818 0.050 Uiso 1 1 calc R . . N2 N 0.26025(19) 0.6070(3) 0.45268(19) 0.0539(10) Uani 1 1 d . . . N4 N 0.03113(17) -0.0921(4) 0.14504(18) 0.0527(10) Uani 1 1 d . . . C10 C 0.3191(2) 0.4618(4) 0.4418(2) 0.0502(12) Uani 1 1 d . . . H10 H 0.3548 0.4294 0.4554 0.060 Uiso 1 1 calc R . . C12 C 0.23905(19) 0.2708(3) 0.3171(2) 0.0401(10) Uani 1 1 d . . . H12A H 0.2253 0.3156 0.2797 0.048 Uiso 1 1 calc R . . H12B H 0.2079 0.2577 0.3289 0.048 Uiso 1 1 calc R . . N1 N 0.40137(18) -0.2130(4) 0.5035(2) 0.0563(11) Uani 1 1 d . . . C25 C 0.26327(18) 0.1591(3) 0.30674(19) 0.0361(9) Uani 1 1 d . . . C3 C 0.33552(19) -0.0757(4) 0.4068(2) 0.0437(10) Uani 1 1 d . . . C8 C 0.2211(2) 0.4708(4) 0.3724(2) 0.0444(11) Uani 1 1 d . . . H8 H 0.1898 0.4444 0.3387 0.053 Uiso 1 1 calc R . . C11 C 0.3097(2) 0.5563(4) 0.4708(2) 0.0517(12) Uani 1 1 d . . . H11 H 0.3399 0.5851 0.5049 0.062 Uiso 1 1 calc R . . C16 C 0.3865(2) 0.2112(5) 0.2294(2) 0.0552(12) Uani 1 1 d . . . H16 H 0.4004 0.1619 0.2626 0.066 Uiso 1 1 calc R . . N3 N 0.4010(2) 0.3017(5) 0.1479(2) 0.0745(15) Uani 1 1 d . . . C15 C 0.33436(19) 0.2649(4) 0.2130(2) 0.0428(10) Uani 1 1 d . . . C23 C 0.0783(2) -0.0879(4) 0.1369(2) 0.0474(11) Uani 1 1 d . . . H23 H 0.0803 -0.1292 0.1047 0.057 Uiso 1 1 calc R . . C14 C 0.3173(2) 0.3390(4) 0.1644(2) 0.0535(12) Uani 1 1 d . . . H14 H 0.2829 0.3764 0.1520 0.064 Uiso 1 1 calc R . . C7 C 0.2176(2) 0.5629(4) 0.4047(2) 0.0564(13) Uani 1 1 d . . . H7 H 0.1824 0.5976 0.3920 0.068 Uiso 1 1 calc R . . C20 C 0.0746(2) 0.0284(5) 0.2321(2) 0.0604(14) Uani 1 1 d . . . H20 H 0.0721 0.0666 0.2649 0.072 Uiso 1 1 calc R . . C19 C 0.0303(2) -0.0341(5) 0.1925(3) 0.0631(14) Uani 1 1 d . . . H19 H -0.0027 -0.0363 0.1991 0.076 Uiso 1 1 calc R . . C5 C 0.3949(2) -0.2343(4) 0.4449(2) 0.0600(14) Uani 1 1 d . . . H5 H 0.4132 -0.2960 0.4376 0.072 Uiso 1 1 calc R . . C17 C 0.4160(3) 0.2336(6) 0.1953(3) 0.0696(16) Uani 1 1 d . . . H17 H 0.4505 0.1971 0.2066 0.084 Uiso 1 1 calc R . . C4 C 0.3629(2) -0.1689(4) 0.3970(2) 0.0555(13) Uani 1 1 d . . . H4 H 0.3591 -0.1861 0.3574 0.067 Uiso 1 1 calc R . . C1 C 0.3748(2) -0.1244(5) 0.5114(2) 0.0600(13) Uani 1 1 d . . . H1 H 0.3790 -0.1086 0.5513 0.072 Uiso 1 1 calc R . . C2 C 0.3414(2) -0.0539(4) 0.4657(2) 0.0523(12) Uani 1 1 d . . . H2 H 0.3233 0.0068 0.4743 0.063 Uiso 1 1 calc R . . C13 C 0.3517(3) 0.3567(5) 0.1343(3) 0.0624(14) Uani 1 1 d . . . H13 H 0.3406 0.4096 0.1028 0.075 Uiso 1 1 calc R . . O5 O 0.4613(4) 0.5297(8) 0.4971(4) 0.175(3) Uiso 1 1 d D . . N5 N 0.4937(6) 0.4414(13) 0.5150(8) 0.135(5) Uiso 0.50 1 d PD . . O6 O 0.4730(9) 0.3732(14) 0.5422(9) 0.205(8) Uiso 0.50 1 d PD . . O7 O 0.4634(14) 0.083(3) 0.4206(12) 0.59(2) Uiso 1 1 d DU . . O8 O 0.4301(10) 0.198(2) 0.4701(13) 0.438(13) Uiso 1 1 d DU . . O9 O 0.5025(19) 0.102(5) 0.5254(12) 1.08(5) Uiso 1 1 d DU . . N6 N 0.4667(10) 0.126(2) 0.4710(10) 1.02(4) Uiso 1 1 d DU . . 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 0.0560(3) 0.0795(3) 0.0534(3) 0.0154(2) 0.0132(2) 0.0244(2) Ag2 0.1006(5) 0.0517(4) 0.0697(4) -0.0247(3) 0.0374(4) 0.0066(3) O2 0.0415(17) 0.0367(15) 0.0517(18) -0.0153(13) 0.0197(15) -0.0010(13) O4 0.0417(18) 0.0539(19) 0.0437(17) -0.0193(14) 0.0209(14) -0.0119(14) O1 0.061(2) 0.0358(16) 0.0394(17) 0.0005(13) 0.0163(15) 0.0066(14) O3 0.0447(18) 0.0465(18) 0.0544(19) 0.0089(14) 0.0260(16) 0.0034(14) C9 0.059(3) 0.033(2) 0.039(2) -0.0085(18) 0.027(2) -0.010(2) C21 0.039(2) 0.044(2) 0.037(2) -0.0065(19) 0.0157(19) -0.0061(19) C6 0.051(3) 0.038(2) 0.036(2) -0.0026(18) 0.017(2) -0.001(2) C24 0.035(2) 0.042(2) 0.034(2) -0.0061(17) 0.0121(18) -0.0014(18) C22 0.042(3) 0.055(3) 0.041(2) -0.006(2) 0.019(2) -0.003(2) C18 0.043(3) 0.042(2) 0.040(2) 0.0004(18) 0.018(2) 0.0005(19) N2 0.068(3) 0.042(2) 0.053(2) -0.0098(18) 0.027(2) 0.002(2) N4 0.047(2) 0.066(3) 0.042(2) -0.0076(19) 0.0160(19) -0.012(2) C10 0.053(3) 0.049(3) 0.050(3) -0.012(2) 0.022(2) -0.007(2) C12 0.041(2) 0.033(2) 0.044(2) -0.0056(18) 0.015(2) -0.0009(18) N1 0.050(3) 0.066(3) 0.051(2) 0.015(2) 0.018(2) 0.014(2) C25 0.039(2) 0.033(2) 0.036(2) -0.0056(17) 0.0147(18) -0.0022(17) C3 0.042(3) 0.042(2) 0.044(2) 0.0055(19) 0.014(2) 0.003(2) C8 0.048(3) 0.038(2) 0.044(2) -0.0040(19) 0.016(2) 0.006(2) C11 0.060(3) 0.049(3) 0.048(3) -0.016(2) 0.024(2) -0.011(2) C16 0.050(3) 0.069(3) 0.048(3) 0.003(2) 0.022(2) 0.001(3) N3 0.074(4) 0.107(4) 0.054(3) -0.008(3) 0.039(3) -0.020(3) C15 0.041(3) 0.046(3) 0.041(2) -0.007(2) 0.018(2) -0.008(2) C23 0.045(3) 0.058(3) 0.038(2) -0.011(2) 0.017(2) -0.001(2) C14 0.057(3) 0.052(3) 0.053(3) -0.002(2) 0.024(3) -0.005(2) C7 0.070(4) 0.046(3) 0.054(3) 0.002(2) 0.026(3) 0.008(2) C20 0.048(3) 0.087(4) 0.053(3) -0.032(3) 0.028(2) -0.015(3) C19 0.050(3) 0.086(4) 0.060(3) -0.021(3) 0.030(3) -0.017(3) C5 0.067(4) 0.055(3) 0.053(3) 0.001(2) 0.019(3) 0.011(3) C17 0.048(3) 0.097(5) 0.066(4) -0.001(3) 0.026(3) -0.002(3) C4 0.066(3) 0.052(3) 0.046(3) 0.001(2) 0.020(2) 0.015(2) C1 0.062(3) 0.074(4) 0.046(3) 0.007(3) 0.025(3) 0.015(3) C2 0.060(3) 0.054(3) 0.046(3) 0.006(2) 0.025(2) 0.011(2) C13 0.067(4) 0.077(4) 0.049(3) 0.002(3) 0.029(3) -0.009(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 N4 2.196(4) 8_546 ? Ag1 N1 2.197(4) . ? Ag1 N3 2.515(5) 6_556 ? Ag2 N2 2.120(4) . ? Ag2 N2 2.120(4) 7_566 ? O2 C9 1.346(5) . ? O2 C12 1.438(5) . ? O4 C21 1.359(5) . ? O4 C24 1.423(5) . ? O1 C3 1.367(5) . ? O1 C6 1.429(5) . ? O3 C15 1.345(5) . ? O3 C18 1.452(5) . ? C9 C10 1.385(6) . ? C9 C8 1.390(6) . ? C21 C22 1.371(6) . ? C21 C20 1.377(6) . ? C6 C25 1.524(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C24 C25 1.530(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C22 C23 1.360(6) . ? C22 H22 0.9300 . ? C18 C25 1.523(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? N2 C11 1.317(7) . ? N2 C7 1.328(7) . ? N4 C23 1.313(6) . ? N4 C19 1.332(6) . ? N4 Ag1 2.196(4) 8_445 ? C10 C11 1.395(7) . ? C10 H10 0.9300 . ? C12 C25 1.537(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N1 C1 1.317(7) . ? N1 C5 1.359(7) . ? C3 C2 1.370(7) . ? C3 C4 1.390(7) . ? C8 C7 1.365(7) . ? C8 H8 0.9300 . ? C11 H11 0.9300 . ? C16 C17 1.351(8) . ? C16 C15 1.397(7) . ? C16 H16 0.9300 . ? N3 C17 1.311(8) . ? N3 C13 1.350(8) . ? N3 Ag1 2.515(5) 6 ? C15 C14 1.377(7) . ? C23 H23 0.9300 . ? C14 C13 1.371(7) . ? C14 H14 0.9300 . ? C7 H7 0.9300 . ? C20 C19 1.368(7) . ? C20 H20 0.9300 . ? C19 H19 0.9300 . ? C5 C4 1.347(7) . ? C5 H5 0.9300 . ? C17 H17 0.9300 . ? C4 H4 0.9300 . ? C1 C2 1.363(7) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C13 H13 0.9300 . ? O5 N5 1.305(9) . ? O5 N5 1.357(15) 5_666 ? N5 O6 1.286(9) . ? N5 O5 1.357(15) 5_666 ? N5 N5 1.66(3) 5_666 ? O7 N6 1.275(10) . ? O8 N6 1.280(10) . ? O9 N6 1.274(10) . ? 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 N4 Ag1 N1 159.96(16) 8_546 . ? N4 Ag1 N3 100.59(16) 8_546 6_556 ? N1 Ag1 N3 99.42(16) . 6_556 ? N2 Ag2 N2 180.0(2) . 7_566 ? C9 O2 C12 119.0(3) . . ? C21 O4 C24 117.1(3) . . ? C3 O1 C6 117.6(3) . . ? C15 O3 C18 117.7(4) . . ? O2 C9 C10 115.4(4) . . ? O2 C9 C8 125.4(4) . . ? C10 C9 C8 119.2(4) . . ? O4 C21 C22 125.1(4) . . ? O4 C21 C20 116.8(4) . . ? C22 C21 C20 118.1(4) . . ? O1 C6 C25 107.4(3) . . ? O1 C6 H6A 110.2 . . ? C25 C6 H6A 110.2 . . ? O1 C6 H6B 110.2 . . ? C25 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? O4 C24 C25 108.8(3) . . ? O4 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? O4 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C23 C22 C21 119.6(4) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? O3 C18 C25 107.3(3) . . ? O3 C18 H18A 110.2 . . ? C25 C18 H18A 110.2 . . ? O3 C18 H18B 110.2 . . ? C25 C18 H18B 110.2 . . ? H18A C18 H18B 108.5 . . ? C11 N2 C7 116.9(4) . . ? C11 N2 Ag2 120.9(3) . . ? C7 N2 Ag2 122.3(4) . . ? C23 N4 C19 116.5(4) . . ? C23 N4 Ag1 121.9(3) . 8_445 ? C19 N4 Ag1 121.5(3) . 8_445 ? C9 C10 C11 117.8(5) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? O2 C12 C25 106.2(3) . . ? O2 C12 H12A 110.5 . . ? C25 C12 H12A 110.5 . . ? O2 C12 H12B 110.5 . . ? C25 C12 H12B 110.5 . . ? H12A C12 H12B 108.7 . . ? C1 N1 C5 116.5(4) . . ? C1 N1 Ag1 120.0(3) . . ? C5 N1 Ag1 123.4(3) . . ? C18 C25 C6 107.7(4) . . ? C18 C25 C24 108.4(3) . . ? C6 C25 C24 111.2(3) . . ? C18 C25 C12 112.4(3) . . ? C6 C25 C12 107.8(3) . . ? C24 C25 C12 109.4(3) . . ? O1 C3 C2 125.1(4) . . ? O1 C3 C4 116.6(4) . . ? C2 C3 C4 118.3(4) . . ? C7 C8 C9 117.2(4) . . ? C7 C8 H8 121.4 . . ? C9 C8 H8 121.4 . . ? N2 C11 C10 123.6(5) . . ? N2 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? C17 C16 C15 117.6(5) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C17 N3 C13 115.1(5) . . ? C17 N3 Ag1 120.5(5) . 6 ? C13 N3 Ag1 124.1(4) . 6 ? O3 C15 C14 115.7(4) . . ? O3 C15 C16 126.5(4) . . ? C14 C15 C16 117.9(4) . . ? N4 C23 C22 123.6(4) . . ? N4 C23 H23 118.2 . . ? C22 C23 H23 118.2 . . ? C13 C14 C15 119.1(5) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? N2 C7 C8 125.3(5) . . ? N2 C7 H7 117.4 . . ? C8 C7 H7 117.4 . . ? C19 C20 C21 117.8(4) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? N4 C19 C20 124.3(5) . . ? N4 C19 H19 117.8 . . ? C20 C19 H19 117.8 . . ? C4 C5 N1 122.1(5) . . ? C4 C5 H5 118.9 . . ? N1 C5 H5 118.9 . . ? N3 C17 C16 126.7(6) . . ? N3 C17 H17 116.6 . . ? C16 C17 H17 116.6 . . ? C5 C4 C3 120.1(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C1 C2 125.4(5) . . ? N1 C1 H1 117.3 . . ? C2 C1 H1 117.3 . . ? C1 C2 C3 117.7(5) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? N3 C13 C14 123.6(5) . . ? N3 C13 H13 118.2 . . ? C14 C13 H13 118.2 . . ? N5 O5 N5 77.3(14) . 5_666 ? O6 N5 O5 109.2(13) . . ? O6 N5 O5 147.2(17) . 5_666 ? O5 N5 O5 102.7(14) . 5_666 ? O6 N5 N5 160.8(17) . 5_666 ? O5 N5 N5 52.8(8) . 5_666 ? O5 N5 N5 50.0(9) 5_666 5_666 ? O9 N6 O7 127.4(17) . . ? O9 N6 O8 112.9(15) . . ? O7 N6 O8 119.7(16) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.042 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.107 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.377 -0.250 0.127 856.0 246.1 2 0.389 0.250 0.639 856.1 246.1 _platon_squeeze_details ; ; #==================================================================== data_compound2 _database_code_depnum_ccdc_archive 'CCDC 875529' #TrackingRef '- p.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H32 Ag2 N6 O14' _chemical_formula_weight 856.31 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 tetragonal _symmetry_space_group_name_H-M 'P -4 2 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z+1/2' '-x, y, -z+1/2' 'y, x, z+1/2' '-y, -x, z+1/2' '-y, x, -z' 'y, -x, -z' _cell_length_a 10.0372(9) _cell_length_b 10.0372(9) _cell_length_c 17.607(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1773.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7993 _exptl_absorpt_correction_T_max 0.8917 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 'Oxford Gemini S Ultra' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1273 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 24.05 _reflns_number_total 1273 _reflns_number_gt 1056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.16(09) _refine_ls_number_reflns 1273 _refine_ls_number_parameters 106 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_ref 0.2046 _refine_ls_wR_factor_gt 0.1966 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.002 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 0.29786(16) 0.0000 0.7500 0.1393(7) Uani 1 2 d S . . C7 C 0.5000 0.5000 1.0000 0.074(3) Uani 1 4 d S . . N1 N 0.3128(8) 0.0240(7) 0.8697(6) 0.109(2) Uani 1 1 d . . . C2 C 0.3850(6) 0.1593(6) 0.9724(5) 0.081(2) Uani 1 1 d . . . C3 C 0.3399(9) 0.0679(8) 1.0249(7) 0.094(2) Uani 1 1 d . . . H3A H 0.3458 0.0831 1.0769 0.113 Uiso 1 1 calc R . . C6 C 0.4664(6) 0.3807(6) 0.9509(4) 0.0751(15) Uani 1 1 d . . . H6A H 0.3898 0.3998 0.9191 0.090 Uiso 1 1 calc R . . H6B H 0.5411 0.3578 0.9185 0.090 Uiso 1 1 calc R . . C4 C 0.2856(10) -0.0478(9) 0.9957(9) 0.109(3) Uani 1 1 d . . . H4A H 0.2557 -0.1141 1.0285 0.131 Uiso 1 1 calc R . . C1 C 0.3705(7) 0.1355(7) 0.8967(6) 0.088(2) Uani 1 1 d . . . H1A H 0.4016 0.1986 0.8623 0.105 Uiso 1 1 calc R . . C5 C 0.2755(11) -0.0650(9) 0.9192(8) 0.112(3) Uani 1 1 d . . . H5A H 0.2402 -0.1447 0.9013 0.134 Uiso 1 1 calc R . . O1 O 0.4375(6) 0.2746(5) 1.0018(4) 0.0923(15) Uani 1 1 d . . . N2 N 0.0000 0.1239(10) 0.7500 0.79(3) Uani 1 2 d SDU . . O2 O 0.092(2) 0.206(2) 0.744(6) 0.74(3) Uani 1 1 d DU . . O1W O 0.382(4) 0.306(2) 0.7269(7) 0.45(4) Uani 1 1 d . . . H1WA H 0.3037 0.3376 0.7225 0.540 Uiso 1 1 d R . . H1WB H 0.4090 0.3495 0.7654 0.540 Uiso 1 1 d R . . O3 O 0.0000 0.0000 0.7500 0.79(3) Uani 1 4 d SDU . . 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 0.1540(11) 0.1024(8) 0.1615(12) -0.0539(8) 0.000 0.000 C7 0.063(4) 0.063(4) 0.096(7) 0.000 0.000 0.000 N1 0.095(4) 0.057(4) 0.174(7) -0.017(4) 0.010(5) -0.001(4) C2 0.057(3) 0.054(3) 0.133(7) -0.004(4) 0.003(3) 0.006(2) C3 0.086(5) 0.060(4) 0.137(6) 0.011(4) -0.001(5) 0.007(3) C6 0.067(4) 0.060(3) 0.099(4) 0.004(3) -0.001(3) -0.002(3) C4 0.085(5) 0.061(4) 0.182(11) 0.016(5) 0.006(6) -0.002(3) C1 0.069(4) 0.062(4) 0.132(7) -0.011(4) 0.007(4) 0.006(3) C5 0.095(6) 0.066(4) 0.174(10) -0.020(5) 0.003(7) -0.010(4) O1 0.097(3) 0.057(2) 0.122(4) 0.007(3) -0.009(3) -0.006(2) N2 0.43(5) 0.31(4) 1.62(8) 0.000 0.01(4) 0.000 O2 0.39(4) 0.27(3) 1.58(8) -0.08(5) 0.11(7) 0.05(3) O1W 0.96(11) 0.235(17) 0.155(12) -0.016(12) 0.18(3) -0.12(3) O3 0.43(6) 0.31(4) 1.62(9) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.127(10) . ? Ag1 N1 2.127(10) 3_556 ? C7 C6 1.515(6) 7_657 ? C7 C6 1.515(6) . ? C7 C6 1.515(6) 8_567 ? C7 C6 1.515(6) 2_665 ? N1 C5 1.303(16) . ? N1 C1 1.346(11) . ? C2 O1 1.372(9) . ? C2 C1 1.363(14) . ? C2 C3 1.379(13) . ? C3 C4 1.381(15) . ? C3 H3A 0.9300 . ? C6 O1 1.421(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C4 C5 1.362(19) . ? C4 H4A 0.9300 . ? C1 H1A 0.9300 . ? C5 H5A 0.9300 . ? N2 O2 1.240(9) . ? N2 O2 1.240(9) 4_556 ? N2 O3 1.244(10) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O3 N2 1.244(10) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 171.9(5) . 3_556 ? C6 C7 C6 109.0(3) 7_657 . ? C6 C7 C6 110.4(5) 7_657 8_567 ? C6 C7 C6 109.0(3) . 8_567 ? C6 C7 C6 109.0(3) 7_657 2_665 ? C6 C7 C6 110.4(5) . 2_665 ? C6 C7 C6 109.0(3) 8_567 2_665 ? C5 N1 C1 117.2(10) . . ? C5 N1 Ag1 124.4(7) . . ? C1 N1 Ag1 118.3(7) . . ? O1 C2 C1 123.9(8) . . ? O1 C2 C3 115.8(8) . . ? C1 C2 C3 120.2(8) . . ? C2 C3 C4 116.1(10) . . ? C2 C3 H3A 121.9 . . ? C4 C3 H3A 121.9 . . ? O1 C6 C7 106.1(5) . . ? O1 C6 H6A 110.5 . . ? C7 C6 H6A 110.5 . . ? O1 C6 H6B 110.5 . . ? C7 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C5 C4 C3 120.3(10) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? N1 C1 C2 122.5(9) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? N1 C5 C4 123.6(8) . . ? N1 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? C2 O1 C6 118.2(7) . . ? O2 N2 O2 97(3) . 4_556 ? O2 N2 O3 131.5(14) . . ? O2 N2 O3 131.5(14) 4_556 . ? H1WA O1W H1WB 100.2 . . ? N2 O3 N2 180.000(2) 2 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 N1 C5 -113.4(8) 3_556 . . . ? N1 Ag1 N1 C1 63.1(6) 3_556 . . . ? O1 C2 C3 C4 179.3(7) . . . . ? C1 C2 C3 C4 2.3(11) . . . . ? C6 C7 C6 O1 59.8(6) 7_657 . . . ? C6 C7 C6 O1 -60.7(6) 8_567 . . . ? C6 C7 C6 O1 179.6(6) 2_665 . . . ? C2 C3 C4 C5 -1.7(13) . . . . ? C5 N1 C1 C2 -2.9(12) . . . . ? Ag1 N1 C1 C2 -179.7(6) . . . . ? O1 C2 C1 N1 -176.8(7) . . . . ? C3 C2 C1 N1 0.0(12) . . . . ? C1 N1 C5 C4 3.6(15) . . . . ? Ag1 N1 C5 C4 -179.8(8) . . . . ? C3 C4 C5 N1 -1.3(17) . . . . ? C1 C2 O1 C6 6.5(10) . . . . ? C3 C2 O1 C6 -170.4(7) . . . . ? C7 C6 O1 C2 170.7(5) . . . . ? O2 N2 O3 N2 -84(100) . . . 2 ? O2 N2 O3 N2 96(100) 4_556 . . 2 ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 24.05 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.598 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.103 #_eof #End of Crystallographic Information File