# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wei-Yin Sun.' _publ_contact_author_email sunwy@nju.edu.cn _publ_section_title ; Syntheses, crystal structures and properties of silver(I) and copper(II) complexes with oxazoline-containing tetradentate ligand ; loop_ _publ_author_name 'Yong-Qing Huang.' 'Guang-Xiang Liu.' 'Xia-Ying Zhou.' T.Okamura 'Zhi Su.' 'Jian Fan.' 'Wei-Yin Sun.' 'Jin-Quan Yu.' 'Norikazu Ueyama' # Attachment '- NJ-ART-02-2010-000092R1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 765656' #TrackingRef '- NJ-ART-02-2010-000092R1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ag(L))OTf _chemical_melting_point ? _chemical_formula_moiety ' C22 H26 Ag N4 O2, C F3 O3 S' _chemical_formula_sum 'C23 H26 Ag F3 N4 O5 S' _chemical_formula_weight 635.41 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.642(2) _cell_length_b 25.648(5) _cell_length_c 9.4569(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.89(3) _cell_angle_gamma 90.00 _cell_volume 2556.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3851 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.70 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8650 _exptl_absorpt_correction_T_max 0.9043 _exptl_absorpt_process_details sadabs,bruker(2000) _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 ? _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 12614 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4509 _reflns_number_gt 3452 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The N1 atom is disordered into two positions (N1, N1'). To get reasonable bond length around N1 and N1' atoms, restraints were added to fix the bond distances of C1-N1, C1-N1', C2-N1, C2-N1' using dfix instruction. Another restrain was added to fix the bond distance of C13-N2 using dfix instruction. The thermal factors of N1, N1', C1 and C2 atoms were restrained using simu and delu instructions. ; _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^)+(0.1164P)^2^+3.2422P] 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 4509 _refine_ls_number_parameters 343 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2026 _refine_ls_wR_factor_gt 0.1867 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.042 _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 0.20587(4) 0.39351(2) 1.23329(6) 0.0822(3) Uani 1 1 d . . . C1 C 0.4834(5) 0.0815(4) 0.6898(8) 0.102(2) Uani 1 1 d DU . . C2 C 0.3522(7) 0.0399(4) 0.4997(8) 0.112(2) Uani 1 1 d DU . . C3 C 0.2270(7) 0.0337(4) 0.4117(8) 0.098(3) Uani 1 1 d . . . C4 C 0.1853(8) 0.0695(3) 0.3047(11) 0.114(3) Uani 1 1 d . . . H4 H 0.2330 0.0993 0.2938 0.137 Uiso 1 1 calc R . . C5 C 0.0726(8) 0.0610(3) 0.2141(9) 0.106(3) Uani 1 1 d . . . H5 H 0.0451 0.0852 0.1432 0.128 Uiso 1 1 calc R . . C6 C 0.0019(6) 0.0170(3) 0.2288(7) 0.0763(17) Uani 1 1 d . . . C7 C 0.0441(6) -0.0170(3) 0.3346(7) 0.0888(19) Uani 1 1 d . . . H7 H -0.0036 -0.0466 0.3470 0.107 Uiso 1 1 calc R . . C8 C 0.1565(7) -0.0088(4) 0.4247(8) 0.098(2) Uani 1 1 d . . . H8 H 0.1833 -0.0332 0.4952 0.118 Uiso 1 1 calc R . . C9 C -0.1165(6) 0.0085(3) 0.1324(7) 0.0763(17) Uani 1 1 d . . . C10 C -0.2638(7) 0.0307(3) -0.0477(8) 0.094(2) Uani 1 1 d . . . H10A H -0.2545 0.0252 -0.1472 0.113 Uiso 1 1 calc R . . H10B H -0.3277 0.0573 -0.0418 0.113 Uiso 1 1 calc R . . C11 C -0.2990(7) -0.0190(3) 0.0202(9) 0.102(2) Uani 1 1 d . . . H11A H -0.3776 -0.0150 0.0602 0.123 Uiso 1 1 calc R . . H11B H -0.3088 -0.0472 -0.0489 0.123 Uiso 1 1 calc R . . C12 C 0.4972(6) 0.1367(3) 0.7395(7) 0.090(2) Uani 1 1 d . . . H12A H 0.5815 0.1416 0.7913 0.108 Uiso 1 1 calc R . . H12B H 0.4885 0.1596 0.6571 0.108 Uiso 1 1 calc R . . C13 C 0.4023(7) 0.2079(3) 0.8514(8) 0.0899(19) Uani 1 1 d D . . H13A H 0.3925 0.2244 0.7583 0.108 Uiso 1 1 calc R . . H13B H 0.4839 0.2185 0.9018 0.108 Uiso 1 1 calc R . . C14 C 0.3002(6) 0.2275(3) 0.9319(6) 0.0762(16) Uani 1 1 d . . . C15 C 0.2296(7) 0.1972(3) 1.0131(7) 0.0817(17) Uani 1 1 d . . . H15 H 0.2448 0.1616 1.0200 0.098 Uiso 1 1 calc R . . C16 C 0.1374(7) 0.2188(3) 1.0839(7) 0.0833(18) Uani 1 1 d . . . H16 H 0.0894 0.1977 1.1360 0.100 Uiso 1 1 calc R . . C17 C 0.1168(6) 0.2717(3) 1.0771(6) 0.0748(16) Uani 1 1 d . . . C18 C 0.1852(7) 0.3017(3) 0.9945(7) 0.0869(19) Uani 1 1 d . . . H18 H 0.1689 0.3373 0.9857 0.104 Uiso 1 1 calc R . . C19 C 0.2766(8) 0.2802(3) 0.9254(7) 0.0864(19) Uani 1 1 d . . . H19 H 0.3237 0.3015 0.8728 0.104 Uiso 1 1 calc R . . C20 C 0.0257(6) 0.2963(3) 1.1606(7) 0.0814(17) Uani 1 1 d . . . C21 C -0.1419(8) 0.2974(4) 1.2765(13) 0.129(3) Uani 1 1 d . . . H21A H -0.1398 0.2825 1.3711 0.155 Uiso 1 1 calc R . . H21B H -0.2294 0.3001 1.2323 0.155 Uiso 1 1 calc R . . C22 C -0.0774(8) 0.3502(4) 1.2837(11) 0.117(3) Uani 1 1 d . . . H22A H -0.1340 0.3767 1.2376 0.140 Uiso 1 1 calc R . . H22B H -0.0505 0.3604 1.3819 0.140 Uiso 1 1 calc R . . C23 C 0.6858(17) 0.1598(10) 0.263(4) 0.287(17) Uani 1 1 d . . . F1 F 0.6496(16) 0.2064(5) 0.230(2) 0.342(11) Uani 1 1 d . . . F2 F 0.732(2) 0.1670(11) 0.392(3) 0.48(2) Uani 1 1 d . . . F3 F 0.7712(18) 0.1506(6) 0.188(3) 0.466(19) Uani 1 1 d . . . N2 N 0.4030(5) 0.1512(2) 0.8319(5) 0.0797(14) Uani 1 1 d D . . H2A H 0.4288 0.1368 0.9191 0.096 Uiso 1 1 calc R . . N3 N -0.1916(5) -0.0294(2) 0.1340(6) 0.0837(15) Uani 1 1 d . . . N4 N 0.0320(5) 0.3427(2) 1.2074(6) 0.0842(15) Uani 1 1 d . . . O1 O -0.1445(5) 0.04559(19) 0.0336(5) 0.0935(14) Uani 1 1 d . . . O2 O -0.0697(5) 0.2665(2) 1.1912(7) 0.1123(18) Uani 1 1 d . . . O3 O 0.4730(13) 0.1354(4) 0.3193(16) 0.250(6) Uani 1 1 d . . . O4 O 0.5309(12) 0.1128(4) 0.1128(11) 0.216(5) Uani 1 1 d . . . O5 O 0.6328(11) 0.0694(4) 0.2951(12) 0.207(4) Uani 1 1 d . . . S1 S 0.5710(2) 0.11444(9) 0.2505(3) 0.1068(7) Uani 1 1 d . . . N1 N 0.3632(7) 0.0850(4) 0.5872(9) 0.099(2) Uani 0.70 1 d PDU . 1 H1A H 0.3686 0.1119 0.5292 0.119 Uiso 0.70 1 d P A 1 H1B H 0.4760 0.0582 0.7677 0.119 Uiso 0.70 1 d P B 1 H1C H 0.5530 0.0709 0.6422 0.119 Uiso 0.70 1 d P C 1 H2B H 0.4178 0.0381 0.4443 0.119 Uiso 0.70 1 d P D 1 H2C H 0.3638 0.0084 0.5655 0.119 Uiso 0.70 1 d P E 1 N1' N 0.3564(13) 0.0544(10) 0.6478(14) 0.104(2) Uani 0.30 1 d PDU . 2 H1' H 0.3605 0.0253 0.7032 0.125 Uiso 0.30 1 d P F 2 H1X H 0.5298 0.0607 0.7635 0.125 Uiso 0.30 1 d P G 2 H1Y H 0.5272 0.0789 0.6082 0.125 Uiso 0.30 1 d P H 2 H2X H 0.4023 0.0622 0.4580 0.125 Uiso 0.30 1 d P I 2 H2Y H 0.3928 0.0049 0.5049 0.125 Uiso 0.30 1 d P J 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0573(3) 0.0973(4) 0.0898(4) 0.0016(2) 0.0018(2) -0.0101(2) C1 0.053(3) 0.153(5) 0.093(4) -0.051(4) -0.013(3) 0.015(3) C2 0.066(3) 0.158(5) 0.105(4) -0.056(4) -0.016(3) 0.016(3) C3 0.061(4) 0.126(6) 0.097(5) -0.055(5) -0.019(4) 0.020(4) C4 0.085(5) 0.086(5) 0.157(8) -0.050(5) -0.034(5) 0.001(4) C5 0.101(5) 0.076(4) 0.128(6) -0.028(4) -0.037(5) 0.008(4) C6 0.065(3) 0.081(4) 0.075(4) -0.022(3) -0.017(3) 0.016(3) C7 0.070(4) 0.114(5) 0.077(4) -0.013(4) -0.009(3) 0.003(4) C8 0.066(4) 0.152(7) 0.072(4) -0.011(4) -0.009(3) 0.018(5) C9 0.070(4) 0.076(4) 0.075(4) -0.017(3) -0.015(3) 0.011(3) C10 0.083(4) 0.101(5) 0.087(5) -0.008(4) -0.029(4) 0.014(4) C11 0.077(4) 0.110(6) 0.105(5) 0.004(4) -0.040(4) 0.000(4) C12 0.058(3) 0.133(7) 0.079(4) -0.007(4) 0.008(3) 0.002(4) C13 0.088(5) 0.103(5) 0.079(4) -0.012(4) 0.015(4) -0.012(4) C14 0.078(4) 0.090(5) 0.059(3) -0.009(3) 0.003(3) -0.010(3) C15 0.089(4) 0.076(4) 0.081(4) -0.005(3) 0.014(3) -0.001(3) C16 0.089(4) 0.081(4) 0.081(4) -0.003(3) 0.018(3) -0.011(3) C17 0.074(4) 0.081(4) 0.067(4) -0.005(3) 0.000(3) -0.009(3) C18 0.110(5) 0.076(4) 0.074(4) -0.001(3) 0.008(4) -0.006(4) C19 0.108(5) 0.080(5) 0.073(4) -0.002(3) 0.018(4) -0.018(4) C20 0.063(4) 0.090(5) 0.088(4) -0.003(4) -0.001(3) -0.011(3) C21 0.082(5) 0.121(7) 0.193(10) -0.021(7) 0.048(6) -0.019(5) C22 0.085(5) 0.113(6) 0.158(8) -0.019(6) 0.036(5) -0.005(5) C23 0.119(11) 0.22(2) 0.50(4) -0.21(3) -0.023(18) 0.002(12) F1 0.298(15) 0.142(8) 0.61(3) -0.118(12) 0.160(19) -0.065(9) F2 0.44(3) 0.41(3) 0.52(3) -0.21(3) -0.27(3) -0.03(2) F3 0.292(17) 0.204(12) 0.98(6) -0.12(2) 0.36(3) -0.098(12) N2 0.068(3) 0.106(4) 0.064(3) -0.010(3) 0.004(2) -0.003(3) N3 0.074(3) 0.086(4) 0.082(3) -0.010(3) -0.021(3) 0.008(3) N4 0.061(3) 0.087(4) 0.104(4) -0.012(3) 0.010(3) -0.003(3) O1 0.086(3) 0.089(3) 0.095(3) -0.003(3) -0.027(2) 0.007(2) O2 0.082(3) 0.096(4) 0.165(5) -0.025(3) 0.037(3) -0.018(3) O3 0.254(13) 0.173(9) 0.361(16) -0.022(10) 0.181(13) 0.030(9) O4 0.206(10) 0.280(13) 0.137(7) 0.014(7) -0.064(7) -0.012(8) O5 0.217(10) 0.126(6) 0.267(11) 0.024(7) -0.009(9) 0.050(7) S1 0.1022(15) 0.1151(17) 0.0999(15) -0.0137(12) 0.0022(12) 0.0106(12) N1 0.053(3) 0.151(5) 0.087(4) -0.049(3) -0.012(3) 0.016(3) N1' 0.055(3) 0.153(5) 0.097(4) -0.050(4) -0.015(3) 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 Ag1 N4 2.248(5) . ? Ag1 N1' 2.316(19) 4_566 ? Ag1 N3 2.358(6) 2_556 ? Ag1 N1 2.376(8) 4_566 ? Ag1 N2 2.459(5) 4_566 ? C1 C12 1.493(12) . ? C1 N1 1.499(7) . ? C1 N1' 1.523(10) . ? C1 H1B 0.959(10) . ? C1 H1C 0.957(7) . ? C1 H1X 0.958(8) . ? C1 H1Y 0.957(8) . ? C2 N1 1.418(8) . ? C2 N1' 1.444(10) . ? C2 C3 1.479(9) . ? C2 H2B 0.930(8) . ? C2 H2C 1.018(10) . ? C2 H2X 0.908(10) . ? C2 H2Y 0.995(8) . ? C3 C8 1.339(12) . ? C3 C4 1.393(12) . ? C4 C5 1.393(10) . ? C4 H4 0.9300 . ? C5 C6 1.373(11) . ? C5 H5 0.9300 . ? C6 C7 1.358(10) . ? C6 C9 1.467(8) . ? C7 C8 1.385(10) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 N3 1.260(9) . ? C9 O1 1.338(8) . ? C10 O1 1.442(8) . ? C10 C11 1.498(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N3 1.483(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N2 1.466(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N2 1.467(7) . ? C13 C14 1.497(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.373(10) . ? C14 C15 1.384(9) . ? C15 C16 1.378(10) . ? C15 H15 0.9300 . ? C16 C17 1.377(10) . ? C16 H16 0.9300 . ? C17 C18 1.374(9) . ? C17 C20 1.473(10) . ? C18 C19 1.361(10) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 N4 1.269(9) . ? C20 O2 1.334(8) . ? C21 O2 1.427(10) . ? C21 C22 1.515(12) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N4 1.464(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 F3 1.25(3) . ? C23 F2 1.26(4) . ? C23 F1 1.28(3) . ? C23 S1 1.68(2) . ? N2 Ag1 2.459(5) 4_565 ? N2 H2A 0.9100 . ? N3 Ag1 2.358(6) 2_546 ? O3 S1 1.409(10) . ? O4 S1 1.315(9) . ? O5 S1 1.368(8) . ? N1 Ag1 2.376(8) 4_565 ? N1 H1A 0.887(12) . ? N1 H2X 1.466(8) . ? N1' Ag1 2.316(19) 4_565 ? N1' H2C 1.421(18) . ? N1' H1' 0.91(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ag1 N1' 153.5(4) . 4_566 ? N4 Ag1 N3 115.6(2) . 2_556 ? N1' Ag1 N3 78.4(6) 4_566 2_556 ? N4 Ag1 N1 134.9(3) . 4_566 ? N1' Ag1 N1 24.1(5) 4_566 4_566 ? N3 Ag1 N1 102.5(3) 2_556 4_566 ? N4 Ag1 N2 114.7(2) . 4_566 ? N1' Ag1 N2 78.8(3) 4_566 4_566 ? N3 Ag1 N2 107.62(18) 2_556 4_566 ? N1 Ag1 N2 72.3(2) 4_566 4_566 ? C12 C1 N1 100.6(7) . . ? C12 C1 N1' 124.1(10) . . ? N1 C1 N1' 37.9(9) . . ? C12 C1 H1B 111.2(6) . . ? N1 C1 H1B 112.5(8) . . ? N1' C1 H1B 75.7(9) . . ? C12 C1 H1C 111.5(7) . . ? N1 C1 H1C 111.1(6) . . ? N1' C1 H1C 117.7(8) . . ? H1B C1 H1C 109.7(8) . . ? C12 C1 H1X 106.2(5) . . ? N1 C1 H1X 144.5(10) . . ? N1' C1 H1X 106.6(12) . . ? H1B C1 H1X 35.4(3) . . ? H1C C1 H1X 80.3(5) . . ? C12 C1 H1Y 106.3(8) . . ? N1 C1 H1Y 87.1(6) . . ? N1' C1 H1Y 105.8(7) . . ? H1B C1 H1Y 132.7(9) . . ? H1C C1 H1Y 26.8(2) . . ? H1X C1 H1Y 106.8(6) . . ? N1 C2 N1' 40.1(10) . . ? N1 C2 C3 114.4(6) . . ? N1' C2 C3 118.6(8) . . ? N1 C2 H2B 111.2(8) . . ? N1' C2 H2B 129.3(8) . . ? C3 C2 H2B 111.5(7) . . ? N1 C2 H2C 107.3(7) . . ? N1' C2 H2C 68.0(11) . . ? C3 C2 H2C 106.4(8) . . ? H2B C2 H2C 105.5(7) . . ? N1 C2 H2X 74.5(7) . . ? N1' C2 H2X 108.5(9) . . ? C3 C2 H2X 111.2(9) . . ? H2B C2 H2X 41.9(4) . . ? H2C C2 H2X 137.4(8) . . ? N1 C2 H2Y 135.0(7) . . ? N1' C2 H2Y 103.1(12) . . ? C3 C2 H2Y 106.4(7) . . ? H2B C2 H2Y 68.2(5) . . ? H2C C2 H2Y 40.2(4) . . ? H2X C2 H2Y 108.3(7) . . ? C8 C3 C4 118.5(6) . . ? C8 C3 C2 120.6(9) . . ? C4 C3 C2 120.6(9) . . ? C5 C4 C3 120.3(8) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 120.3(8) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C7 C6 C5 118.2(6) . . ? C7 C6 C9 122.1(7) . . ? C5 C6 C9 119.7(6) . . ? C6 C7 C8 121.8(8) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C3 C8 C7 120.9(8) . . ? C3 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? N3 C9 O1 118.4(5) . . ? N3 C9 C6 126.9(6) . . ? O1 C9 C6 114.7(6) . . ? O1 C10 C11 104.5(5) . . ? O1 C10 H10A 110.8 . . ? C11 C10 H10A 110.8 . . ? O1 C10 H10B 110.8 . . ? C11 C10 H10B 110.8 . . ? H10A C10 H10B 108.9 . . ? N3 C11 C10 104.5(6) . . ? N3 C11 H11A 110.9 . . ? C10 C11 H11A 110.9 . . ? N3 C11 H11B 110.9 . . ? C10 C11 H11B 110.9 . . ? H11A C11 H11B 108.9 . . ? N2 C12 C1 112.5(6) . . ? N2 C12 H12A 109.1 . . ? C1 C12 H12A 109.1 . . ? N2 C12 H12B 109.1 . . ? C1 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? N2 C13 C14 114.5(6) . . ? N2 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? N2 C13 H13B 108.6 . . ? C14 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C19 C14 C15 117.8(6) . . ? C19 C14 C13 116.7(6) . . ? C15 C14 C13 125.5(6) . . ? C16 C15 C14 121.5(7) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 119.5(6) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C18 C17 C16 119.0(7) . . ? C18 C17 C20 120.3(6) . . ? C16 C17 C20 120.6(6) . . ? C19 C18 C17 121.1(7) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C14 121.1(7) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? N4 C20 O2 117.8(7) . . ? N4 C20 C17 125.6(6) . . ? O2 C20 C17 116.6(6) . . ? O2 C21 C22 104.2(7) . . ? O2 C21 H21A 110.9 . . ? C22 C21 H21A 110.9 . . ? O2 C21 H21B 110.9 . . ? C22 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? N4 C22 C21 104.3(7) . . ? N4 C22 H22A 110.9 . . ? C21 C22 H22A 110.9 . . ? N4 C22 H22B 110.9 . . ? C21 C22 H22B 110.9 . . ? H22A C22 H22B 108.9 . . ? F3 C23 F2 111(2) . . ? F3 C23 F1 105(4) . . ? F2 C23 F1 99.6(18) . . ? F3 C23 S1 113.9(15) . . ? F2 C23 S1 111(3) . . ? F1 C23 S1 115.9(15) . . ? C12 N2 C13 110.0(6) . . ? C12 N2 Ag1 105.9(4) . 4_565 ? C13 N2 Ag1 119.4(4) . 4_565 ? C12 N2 H2A 107.0 . . ? C13 N2 H2A 107.0 . . ? Ag1 N2 H2A 107.0 4_565 . ? C9 N3 C11 106.3(6) . . ? C9 N3 Ag1 137.8(4) . 2_546 ? C11 N3 Ag1 115.9(5) . 2_546 ? C20 N4 C22 106.7(6) . . ? C20 N4 Ag1 125.8(5) . . ? C22 N4 Ag1 124.7(5) . . ? C9 O1 C10 106.2(6) . . ? C20 O2 C21 106.9(6) . . ? O4 S1 O5 110.8(7) . . ? O4 S1 O3 108.0(9) . . ? O5 S1 O3 122.3(8) . . ? O4 S1 C23 103.2(15) . . ? O5 S1 C23 104.5(11) . . ? O3 S1 C23 106.2(9) . . ? C2 N1 C1 108.8(6) . . ? C2 N1 Ag1 121.3(6) . 4_565 ? C1 N1 Ag1 104.2(5) . 4_565 ? C2 N1 H1A 106.2(8) . . ? C1 N1 H1A 109.0(8) . . ? Ag1 N1 H1A 106.9(5) 4_565 . ? C2 N1 H2X 36.7(5) . . ? C1 N1 H2X 101.5(5) . . ? Ag1 N1 H2X 151.7(4) 4_565 . ? H1A N1 H2X 75.2(6) . . ? C2 N1' C1 106.1(8) . . ? C2 N1' Ag1 123.8(12) . 4_565 ? C1 N1' Ag1 106.1(10) . 4_565 ? C2 N1' H2C 41.6(6) . . ? C1 N1' H2C 114.0(11) . . ? Ag1 N1' H2C 139.8(7) 4_565 . ? C2 N1' H1' 110.0(17) . . ? C1 N1' H1' 104.7(14) . . ? Ag1 N1' H1' 104.6(9) 4_565 . ? H2C N1' H1' 68.5(14) . . ? 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 C2 C3 C8 -120.9(9) . . . . ? N1' C2 C3 C8 -76.1(15) . . . . ? N1 C2 C3 C4 65.0(11) . . . . ? N1' C2 C3 C4 109.8(15) . . . . ? C8 C3 C4 C5 0.1(12) . . . . ? C2 C3 C4 C5 174.3(7) . . . . ? C3 C4 C5 C6 -0.4(13) . . . . ? C4 C5 C6 C7 0.9(11) . . . . ? C4 C5 C6 C9 -179.9(7) . . . . ? C5 C6 C7 C8 -1.2(11) . . . . ? C9 C6 C7 C8 179.6(6) . . . . ? C4 C3 C8 C7 -0.4(11) . . . . ? C2 C3 C8 C7 -174.6(6) . . . . ? C6 C7 C8 C3 1.0(11) . . . . ? C7 C6 C9 N3 0.1(11) . . . . ? C5 C6 C9 N3 -179.1(7) . . . . ? C7 C6 C9 O1 -179.8(6) . . . . ? C5 C6 C9 O1 1.0(9) . . . . ? O1 C10 C11 N3 -2.0(8) . . . . ? N1 C1 C12 N2 71.2(8) . . . . ? N1' C1 C12 N2 38.6(12) . . . . ? N2 C13 C14 C19 -165.6(6) . . . . ? N2 C13 C14 C15 15.3(10) . . . . ? C19 C14 C15 C16 0.8(10) . . . . ? C13 C14 C15 C16 179.9(7) . . . . ? C14 C15 C16 C17 -1.7(11) . . . . ? C15 C16 C17 C18 2.7(10) . . . . ? C15 C16 C17 C20 -175.3(6) . . . . ? C16 C17 C18 C19 -3.1(10) . . . . ? C20 C17 C18 C19 174.9(7) . . . . ? C17 C18 C19 C14 2.3(11) . . . . ? C15 C14 C19 C18 -1.1(10) . . . . ? C13 C14 C19 C18 179.7(7) . . . . ? C18 C17 C20 N4 -26.8(10) . . . . ? C16 C17 C20 N4 151.1(7) . . . . ? C18 C17 C20 O2 154.5(7) . . . . ? C16 C17 C20 O2 -27.5(9) . . . . ? O2 C21 C22 N4 -3.5(11) . . . . ? C1 C12 N2 C13 -167.5(6) . . . . ? C1 C12 N2 Ag1 -37.2(6) . . . 4_565 ? C14 C13 N2 C12 174.0(6) . . . . ? C14 C13 N2 Ag1 51.4(7) . . . 4_565 ? O1 C9 N3 C11 -2.4(9) . . . . ? C6 C9 N3 C11 177.7(7) . . . . ? O1 C9 N3 Ag1 179.2(5) . . . 2_546 ? C6 C9 N3 Ag1 -0.7(11) . . . 2_546 ? C10 C11 N3 C9 2.6(8) . . . . ? C10 C11 N3 Ag1 -178.6(5) . . . 2_546 ? O2 C20 N4 C22 -1.3(9) . . . . ? C17 C20 N4 C22 180.0(7) . . . . ? O2 C20 N4 Ag1 160.1(5) . . . . ? C17 C20 N4 Ag1 -18.5(10) . . . . ? C21 C22 N4 C20 3.0(10) . . . . ? C21 C22 N4 Ag1 -158.8(6) . . . . ? N1' Ag1 N4 C20 74.4(13) 4_566 . . . ? N3 Ag1 N4 C20 -168.1(6) 2_556 . . . ? N1 Ag1 N4 C20 47.2(8) 4_566 . . . ? N2 Ag1 N4 C20 -42.0(7) 4_566 . . . ? N1' Ag1 N4 C22 -127.3(12) 4_566 . . . ? N3 Ag1 N4 C22 -9.8(7) 2_556 . . . ? N1 Ag1 N4 C22 -154.5(7) 4_566 . . . ? N2 Ag1 N4 C22 116.3(7) 4_566 . . . ? N3 C9 O1 C10 1.1(8) . . . . ? C6 C9 O1 C10 -179.0(6) . . . . ? C11 C10 O1 C9 0.7(8) . . . . ? N4 C20 O2 C21 -1.0(10) . . . . ? C17 C20 O2 C21 177.7(7) . . . . ? C22 C21 O2 C20 2.8(11) . . . . ? F3 C23 S1 O4 -56(3) . . . . ? F2 C23 S1 O4 178(2) . . . . ? F1 C23 S1 O4 66(3) . . . . ? F3 C23 S1 O5 60(3) . . . . ? F2 C23 S1 O5 -66(2) . . . . ? F1 C23 S1 O5 -178(3) . . . . ? F3 C23 S1 O3 -169(3) . . . . ? F2 C23 S1 O3 65(2) . . . . ? F1 C23 S1 O3 -48(3) . . . . ? N1' C2 N1 C1 63.1(10) . . . . ? C3 C2 N1 C1 169.3(9) . . . . ? N1' C2 N1 Ag1 -57.5(12) . . . 4_565 ? C3 C2 N1 Ag1 48.6(11) . . . 4_565 ? C12 C1 N1 C2 164.1(8) . . . . ? N1' C1 N1 C2 -62.4(10) . . . . ? C12 C1 N1 Ag1 -65.1(7) . . . 4_565 ? N1' C1 N1 Ag1 68.3(12) . . . 4_565 ? N1 C2 N1' C1 -59.9(10) . . . . ? C3 C2 N1' C1 -154.6(11) . . . . ? N1 C2 N1' Ag1 62.9(16) . . . 4_565 ? C3 C2 N1' Ag1 -31.8(19) . . . 4_565 ? C12 C1 N1' C2 118.7(13) . . . . ? N1 C1 N1' C2 59.1(10) . . . . ? C12 C1 N1' Ag1 -14.6(14) . . . 4_565 ? N1 C1 N1' Ag1 -74.2(15) . . . 4_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.059 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.107 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 765657' #TrackingRef '- NJ-ART-02-2010-000092R1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H26 Ag F3 N4 O5 S' _chemical_formula_sum 'C23 H26 Ag F3 N4 O5 S' _chemical_formula_weight 635.41 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 monoclinic _symmetry_space_group_name_H-M 'p 21/n' _symmetry_space_group_name_Hall '-p 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.0542(11) _cell_length_b 7.8076(5) _cell_length_c 18.7729(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.7930(10) _cell_angle_gamma 90.00 _cell_volume 2486.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3779 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 23.11 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8312 _exptl_absorpt_correction_T_max 0.8616 _exptl_absorpt_process_details 'sadabs (Bruker, 2001)' _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 'Bruker Smart Apex CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14205 _diffrn_reflns_av_R_equivalents 0.0475 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5655 _reflns_number_gt 4239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _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^)+(0.0896P)^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 5655 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1544 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.47187(2) 0.21455(5) 0.708630(19) 0.05241(17) Uani 1 1 d . . . S1 S 0.66309(9) 0.72984(19) 0.90646(9) 0.0644(4) Uani 1 1 d . . . F1 F 0.6132(5) 0.4812(6) 0.9792(2) 0.166 Uani 1 1 d . . . F2 F 0.5834(5) 0.7245(11) 1.0130(4) 0.205(4) Uani 1 1 d . . . F3 F 0.6972(4) 0.6396(7) 1.0374(2) 0.159 Uani 1 1 d . . . N3 N 0.5267(3) 1.1715(5) 0.5996(2) 0.0561(10) Uani 1 1 d . . . O2 O 0.25793(18) -0.5195(4) 0.60843(17) 0.0530(8) Uani 1 1 d . . . O3 O 0.5918(3) 0.7216(6) 0.8615(2) 0.0844(13) Uani 1 1 d . . . O4 O 0.6903(3) 0.8943(6) 0.9274(3) 0.1054(16) Uani 1 1 d . . . O5 O 0.7223(3) 0.6195(9) 0.8857(4) 0.134(2) Uani 1 1 d . . . N1 N 0.5805(2) 0.3657(5) 0.7735(2) 0.0473(9) Uani 1 1 d . . . H1C H 0.5616 0.4563 0.7969 0.057 Uiso 1 1 calc R . . N2 N 0.49379(19) 0.0508(5) 0.81638(18) 0.0422(8) Uani 1 1 d . . . H2C H 0.5236 -0.0412 0.8066 0.051 Uiso 1 1 calc R . . O1 O 0.6095(2) 1.0886(5) 0.52123(18) 0.0629(9) Uani 1 1 d . . . N4 N 0.3488(2) -0.7010(5) 0.6589(2) 0.0498(9) Uani 1 1 d . . . C1 C 0.6095(3) 0.2355(6) 0.8254(3) 0.0538(12) Uani 1 1 d . . . H1A H 0.6493 0.2855 0.8597 0.065 Uiso 1 1 calc R . . H1B H 0.6339 0.1435 0.8008 0.065 Uiso 1 1 calc R . . C2 C 0.5441(3) 0.1641(6) 0.8642(3) 0.0506(11) Uani 1 1 d . . . H2A H 0.5661 0.1002 0.9058 0.061 Uiso 1 1 calc R . . H2B H 0.5127 0.2571 0.8805 0.061 Uiso 1 1 calc R . . C3 C 0.6416(3) 0.4246(6) 0.7306(3) 0.0522(11) Uani 1 1 d . . . H3A H 0.6536 0.3338 0.6981 0.063 Uiso 1 1 calc R . . H3B H 0.6891 0.4479 0.7621 0.063 Uiso 1 1 calc R . . C4 C 0.4254(3) -0.0150(6) 0.8502(3) 0.0538(12) Uani 1 1 d . . . H4A H 0.3875 0.0762 0.8541 0.065 Uiso 1 1 calc R . . H4B H 0.4424 -0.0561 0.8981 0.065 Uiso 1 1 calc R . . C5 C 0.6192(2) 0.5829(6) 0.6879(2) 0.0454(10) Uani 1 1 d . . . C6 C 0.6723(3) 0.6531(7) 0.6451(3) 0.0539(12) Uani 1 1 d . . . H6A H 0.7194 0.5960 0.6407 0.065 Uiso 1 1 calc R . . C7 C 0.6576(3) 0.8036(6) 0.6092(3) 0.0545(12) Uani 1 1 d . . . H7A H 0.6949 0.8479 0.5813 0.065 Uiso 1 1 calc R . . C8 C 0.5875(2) 0.8911(6) 0.6142(2) 0.0453(10) Uani 1 1 d . . . C9 C 0.5335(3) 0.8180(6) 0.6556(3) 0.0513(12) Uani 1 1 d . . . H9A H 0.4857 0.8730 0.6591 0.062 Uiso 1 1 calc R . . C10 C 0.5485(3) 0.6689(6) 0.6908(3) 0.0497(11) Uani 1 1 d . . . H10A H 0.5106 0.6230 0.7175 0.060 Uiso 1 1 calc R . . C11 C 0.5718(3) 1.0567(6) 0.5795(2) 0.0485(11) Uani 1 1 d . . . C12 C 0.5972(4) 1.2675(8) 0.5072(3) 0.0714(16) Uani 1 1 d . . . H12A H 0.5858 1.2886 0.4563 0.086 Uiso 1 1 calc R . . H12B H 0.6432 1.3338 0.5250 0.086 Uiso 1 1 calc R . . C13 C 0.5278(4) 1.3116(7) 0.5467(3) 0.0648(15) Uani 1 1 d . . . H13A H 0.5348 1.4219 0.5702 0.078 Uiso 1 1 calc R . . H13B H 0.4794 1.3134 0.5146 0.078 Uiso 1 1 calc R . . C14 C 0.3877(3) -0.1592(6) 0.8056(2) 0.0451(10) Uani 1 1 d . . . C15 C 0.4006(3) -0.3275(6) 0.8255(2) 0.0471(11) Uani 1 1 d . . . H15A H 0.4273 -0.3531 0.8698 0.057 Uiso 1 1 calc R . . C16 C 0.3738(2) -0.4582(6) 0.7797(2) 0.0431(10) Uani 1 1 d . . . H16A H 0.3823 -0.5716 0.7937 0.052 Uiso 1 1 calc R . . C17 C 0.3344(2) -0.4216(6) 0.7129(2) 0.0396(9) Uani 1 1 d . . . C18 C 0.3177(3) -0.2527(6) 0.6959(3) 0.0469(11) Uani 1 1 d . . . H18A H 0.2882 -0.2258 0.6530 0.056 Uiso 1 1 calc R . . C19 C 0.3445(3) -0.1237(6) 0.7421(3) 0.0485(11) Uani 1 1 d . . . H19A H 0.3331 -0.0104 0.7299 0.058 Uiso 1 1 calc R . . C20 C 0.3155(2) -0.5565(6) 0.6611(2) 0.0405(9) Uani 1 1 d . . . C21 C 0.3092(4) -0.7929(7) 0.5958(3) 0.0635(14) Uani 1 1 d . . . H21A H 0.2797 -0.8905 0.6108 0.076 Uiso 1 1 calc R . . H21B H 0.3474 -0.8326 0.5646 0.076 Uiso 1 1 calc R . . C22 C 0.2554(3) -0.6633(7) 0.5589(3) 0.0598(13) Uani 1 1 d . . . H22A H 0.2737 -0.6293 0.5137 0.072 Uiso 1 1 calc R . . H22B H 0.2023 -0.7082 0.5499 0.072 Uiso 1 1 calc R . . C23 C 0.6373(6) 0.6392(10) 0.9868(4) 0.105(3) Uani 1 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 0.0499(2) 0.0495(3) 0.0562(3) -0.00219(16) -0.00242(17) 0.00528(16) S1 0.0598(8) 0.0539(8) 0.0767(9) -0.0054(7) -0.0063(7) 0.0060(6) F1 0.313 0.081 0.101 0.017 0.000 -0.083 F2 0.237(8) 0.265(9) 0.131(5) -0.066(5) 0.110(6) -0.048(6) F3 0.243 0.142 0.075 0.025 -0.071 -0.033 N3 0.075(3) 0.045(2) 0.049(2) 0.0035(18) 0.007(2) 0.003(2) O2 0.0549(18) 0.0443(19) 0.0572(19) -0.0002(15) -0.0072(15) 0.0105(15) O3 0.080(3) 0.084(3) 0.083(3) -0.010(2) -0.022(2) 0.011(2) O4 0.120(4) 0.063(3) 0.129(4) -0.010(3) -0.007(3) -0.031(3) O5 0.098(4) 0.138(5) 0.165(5) -0.041(4) -0.002(4) 0.053(4) N1 0.0429(19) 0.032(2) 0.067(2) -0.0017(17) 0.0057(17) 0.0007(16) N2 0.0446(19) 0.0309(19) 0.051(2) -0.0033(16) 0.0050(16) -0.0003(15) O1 0.072(2) 0.061(2) 0.058(2) 0.0030(17) 0.0148(17) -0.0040(19) N4 0.050(2) 0.038(2) 0.060(2) -0.0046(17) -0.0042(18) 0.0046(18) C1 0.046(3) 0.044(3) 0.068(3) -0.001(2) -0.007(2) -0.001(2) C2 0.053(3) 0.043(3) 0.053(3) -0.003(2) -0.008(2) -0.001(2) C3 0.039(2) 0.043(3) 0.075(3) -0.005(2) 0.011(2) -0.003(2) C4 0.058(3) 0.042(3) 0.062(3) -0.007(2) 0.012(2) -0.008(2) C5 0.039(2) 0.041(3) 0.058(3) -0.013(2) 0.0074(19) -0.0081(19) C6 0.038(2) 0.049(3) 0.076(3) -0.006(3) 0.010(2) -0.001(2) C7 0.044(3) 0.053(3) 0.069(3) -0.005(2) 0.016(2) -0.012(2) C8 0.045(2) 0.040(3) 0.051(3) -0.0084(19) 0.0042(19) -0.007(2) C9 0.044(2) 0.046(3) 0.066(3) -0.008(2) 0.014(2) 0.003(2) C10 0.044(2) 0.043(3) 0.064(3) -0.001(2) 0.016(2) -0.003(2) C11 0.049(2) 0.048(3) 0.049(3) -0.008(2) 0.005(2) -0.012(2) C12 0.089(4) 0.067(4) 0.057(3) 0.015(3) -0.001(3) -0.011(3) C13 0.089(4) 0.048(3) 0.054(3) 0.008(2) -0.007(3) -0.002(3) C14 0.043(2) 0.040(2) 0.054(3) -0.004(2) 0.013(2) -0.004(2) C15 0.048(2) 0.044(3) 0.050(3) 0.003(2) 0.007(2) -0.004(2) C16 0.047(2) 0.036(2) 0.046(2) 0.0015(19) 0.0064(19) 0.0018(19) C17 0.0322(19) 0.036(2) 0.052(2) 0.0003(19) 0.0127(17) 0.0016(17) C18 0.043(2) 0.038(3) 0.058(3) 0.006(2) 0.003(2) 0.0032(19) C19 0.050(2) 0.033(2) 0.063(3) -0.001(2) 0.008(2) 0.001(2) C20 0.035(2) 0.038(2) 0.049(2) 0.0051(19) 0.0051(17) -0.0001(18) C21 0.067(3) 0.046(3) 0.074(4) -0.012(3) -0.011(3) 0.006(3) C22 0.063(3) 0.057(3) 0.056(3) -0.008(2) -0.006(2) 0.001(3) C23 0.177(8) 0.069(5) 0.066(4) -0.012(3) -0.002(5) -0.032(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 Ag1 N4 2.306(4) 1_565 ? Ag1 N3 2.360(4) 1_545 ? Ag1 N2 2.390(4) . ? Ag1 N1 2.419(4) . ? S1 O4 1.408(5) . ? S1 O3 1.410(4) . ? S1 O5 1.412(5) . ? S1 C23 1.762(8) . ? F1 C23 1.303(8) . ? F2 C23 1.273(11) . ? F3 C23 1.322(9) . ? N3 C11 1.263(6) . ? N3 C13 1.479(6) . ? N3 Ag1 2.360(4) 1_565 ? O2 C20 1.352(5) . ? O2 C22 1.456(6) . ? N1 C1 1.459(6) . ? N1 C3 1.454(6) . ? N1 H1C 0.9100 . ? N2 C2 1.472(6) . ? N2 C4 1.476(5) . ? N2 H2C 0.9100 . ? O1 C11 1.346(5) . ? O1 C12 1.433(7) . ? N4 C20 1.266(6) . ? N4 C21 1.486(6) . ? N4 Ag1 2.306(4) 1_545 ? C1 C2 1.499(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C5 1.501(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C14 1.509(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.383(6) . ? C5 C10 1.385(6) . ? C6 C7 1.365(7) . ? C6 H6A 0.9300 . ? C7 C8 1.388(6) . ? C7 H7A 0.9300 . ? C8 C9 1.387(6) . ? C8 C11 1.460(7) . ? C9 C10 1.350(7) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C12 C13 1.499(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.378(7) . ? C14 C19 1.364(6) . ? C15 C16 1.381(6) . ? C15 H15A 0.9300 . ? C16 C17 1.392(6) . ? C16 H16A 0.9300 . ? C17 C18 1.380(6) . ? C17 C20 1.448(6) . ? C18 C19 1.377(6) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C22 1.488(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? 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 N3 96.52(15) 1_565 1_545 ? N4 Ag1 N2 123.64(13) 1_565 . ? N3 Ag1 N2 128.05(13) 1_545 . ? N4 Ag1 N1 133.18(13) 1_565 . ? N3 Ag1 N1 98.94(14) 1_545 . ? N2 Ag1 N1 77.80(12) . . ? O4 S1 O3 116.7(3) . . ? O4 S1 O5 114.1(4) . . ? O3 S1 O5 113.8(3) . . ? O4 S1 C23 103.3(3) . . ? O3 S1 C23 102.7(4) . . ? O5 S1 C23 103.8(5) . . ? C11 N3 C13 106.0(4) . . ? C11 N3 Ag1 131.8(3) . 1_565 ? C13 N3 Ag1 120.7(3) . 1_565 ? C20 O2 C22 105.9(3) . . ? C1 N1 C3 112.1(4) . . ? C1 N1 Ag1 100.8(3) . . ? C3 N1 Ag1 115.6(3) . . ? C1 N1 H1C 109.3 . . ? C3 N1 H1C 109.3 . . ? Ag1 N1 H1C 109.3 . . ? C2 N2 C4 112.6(4) . . ? C2 N2 Ag1 103.1(3) . . ? C4 N2 Ag1 119.2(3) . . ? C2 N2 H2C 107.1 . . ? C4 N2 H2C 107.1 . . ? Ag1 N2 H2C 107.1 . . ? C11 O1 C12 104.9(4) . . ? C20 N4 C21 106.7(4) . . ? C20 N4 Ag1 129.4(3) . 1_545 ? C21 N4 Ag1 120.4(3) . 1_545 ? N1 C1 C2 111.4(4) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 110.1(4) . . ? N2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.2 . . ? N1 C3 C5 113.4(4) . . ? N1 C3 H3A 108.9 . . ? C5 C3 H3A 108.9 . . ? N1 C3 H3B 108.9 . . ? C5 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N2 C4 C14 109.4(4) . . ? N2 C4 H4A 109.8 . . ? C14 C4 H4A 109.8 . . ? N2 C4 H4B 109.8 . . ? C14 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C10 117.0(5) . . ? C6 C5 C3 119.3(4) . . ? C10 C5 C3 123.7(4) . . ? C7 C6 C5 122.0(4) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C6 C7 C8 120.4(4) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C7 C8 C9 117.4(4) . . ? C7 C8 C11 121.8(4) . . ? C9 C8 C11 120.8(4) . . ? C10 C9 C8 121.7(4) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C9 C10 C5 121.4(4) . . ? C9 C10 H10A 119.3 . . ? C5 C10 H10A 119.3 . . ? N3 C11 O1 117.8(5) . . ? N3 C11 C8 125.8(4) . . ? O1 C11 C8 116.4(4) . . ? O1 C12 C13 103.9(4) . . ? O1 C12 H12A 111.0 . . ? C13 C12 H12A 111.0 . . ? O1 C12 H12B 111.0 . . ? C13 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? N3 C13 C12 103.1(4) . . ? N3 C13 H13A 111.2 . . ? C12 C13 H13A 111.2 . . ? N3 C13 H13B 111.2 . . ? C12 C13 H13B 111.2 . . ? H13A C13 H13B 109.1 . . ? C15 C14 C19 119.2(4) . . ? C15 C14 C4 120.9(4) . . ? C19 C14 C4 119.8(4) . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C15 C16 C17 120.5(4) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C18 C17 C16 118.3(4) . . ? C18 C17 C20 120.9(4) . . ? C16 C17 C20 120.7(4) . . ? C19 C18 C17 120.4(4) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C18 C19 C14 121.2(4) . . ? C18 C19 H19A 119.4 . . ? C14 C19 H19A 119.4 . . ? N4 C20 O2 117.5(4) . . ? N4 C20 C17 126.9(4) . . ? O2 C20 C17 115.6(4) . . ? N4 C21 C22 104.6(4) . . ? N4 C21 H21A 110.8 . . ? C22 C21 H21A 110.8 . . ? N4 C21 H21B 110.8 . . ? C22 C21 H21B 110.8 . . ? H21A C21 H21B 108.9 . . ? O2 C22 C21 104.5(4) . . ? O2 C22 H22A 110.9 . . ? C21 C22 H22A 110.9 . . ? O2 C22 H22B 110.9 . . ? C21 C22 H22B 110.9 . . ? H22A C22 H22B 108.9 . . ? F2 C23 F1 107.8(9) . . ? F2 C23 F3 104.9(7) . . ? F1 C23 F3 107.1(7) . . ? F2 C23 S1 111.9(7) . . ? F1 C23 S1 112.9(5) . . ? F3 C23 S1 111.9(7) . . ? 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 N4 Ag1 N1 C1 143.3(3) 1_565 . . . ? N3 Ag1 N1 C1 -108.9(3) 1_545 . . . ? N2 Ag1 N1 C1 18.3(3) . . . . ? N4 Ag1 N1 C3 -95.6(3) 1_565 . . . ? N3 Ag1 N1 C3 12.2(3) 1_545 . . . ? N2 Ag1 N1 C3 139.4(3) . . . . ? N4 Ag1 N2 C2 -119.6(3) 1_565 . . . ? N3 Ag1 N2 C2 106.4(3) 1_545 . . . ? N1 Ag1 N2 C2 14.6(3) . . . . ? N4 Ag1 N2 C4 5.9(4) 1_565 . . . ? N3 Ag1 N2 C4 -128.0(3) 1_545 . . . ? N1 Ag1 N2 C4 140.1(3) . . . . ? C3 N1 C1 C2 -174.6(4) . . . . ? Ag1 N1 C1 C2 -51.1(4) . . . . ? C4 N2 C2 C1 -176.4(4) . . . . ? Ag1 N2 C2 C1 -46.7(4) . . . . ? N1 C1 C2 N2 73.3(5) . . . . ? C1 N1 C3 C5 -167.9(4) . . . . ? Ag1 N1 C3 C5 77.4(4) . . . . ? C2 N2 C4 C14 -167.1(4) . . . . ? Ag1 N2 C4 C14 72.0(4) . . . . ? N1 C3 C5 C6 179.6(4) . . . . ? N1 C3 C5 C10 2.3(6) . . . . ? C10 C5 C6 C7 2.4(7) . . . . ? C3 C5 C6 C7 -175.0(5) . . . . ? C5 C6 C7 C8 -0.7(8) . . . . ? C6 C7 C8 C9 -1.1(7) . . . . ? C6 C7 C8 C11 176.8(5) . . . . ? C7 C8 C9 C10 1.0(7) . . . . ? C11 C8 C9 C10 -176.8(5) . . . . ? C8 C9 C10 C5 0.8(8) . . . . ? C6 C5 C10 C9 -2.5(7) . . . . ? C3 C5 C10 C9 174.9(5) . . . . ? C13 N3 C11 O1 2.3(6) . . . . ? Ag1 N3 C11 O1 -163.2(3) 1_565 . . . ? C13 N3 C11 C8 -178.0(4) . . . . ? Ag1 N3 C11 C8 16.4(7) 1_565 . . . ? C12 O1 C11 N3 11.3(6) . . . . ? C12 O1 C11 C8 -168.4(4) . . . . ? C7 C8 C11 N3 -153.2(5) . . . . ? C9 C8 C11 N3 24.5(7) . . . . ? C7 C8 C11 O1 26.4(6) . . . . ? C9 C8 C11 O1 -155.9(4) . . . . ? C11 O1 C12 C13 -19.1(5) . . . . ? C11 N3 C13 C12 -14.2(6) . . . . ? Ag1 N3 C13 C12 153.3(4) 1_565 . . . ? O1 C12 C13 N3 20.1(6) . . . . ? N2 C4 C14 C15 101.9(5) . . . . ? N2 C4 C14 C19 -73.6(5) . . . . ? C19 C14 C15 C16 3.7(6) . . . . ? C4 C14 C15 C16 -171.9(4) . . . . ? C14 C15 C16 C17 0.6(6) . . . . ? C15 C16 C17 C18 -4.7(6) . . . . ? C15 C16 C17 C20 171.8(4) . . . . ? C16 C17 C18 C19 4.5(6) . . . . ? C20 C17 C18 C19 -172.0(4) . . . . ? C17 C18 C19 C14 -0.3(7) . . . . ? C15 C14 C19 C18 -3.8(6) . . . . ? C4 C14 C19 C18 171.7(4) . . . . ? C21 N4 C20 O2 -2.1(6) . . . . ? Ag1 N4 C20 O2 156.4(3) 1_545 . . . ? C21 N4 C20 C17 -179.4(4) . . . . ? Ag1 N4 C20 C17 -20.9(7) 1_545 . . . ? C22 O2 C20 N4 -4.1(5) . . . . ? C22 O2 C20 C17 173.6(4) . . . . ? C18 C17 C20 N4 154.4(5) . . . . ? C16 C17 C20 N4 -22.0(7) . . . . ? C18 C17 C20 O2 -23.0(5) . . . . ? C16 C17 C20 O2 160.6(4) . . . . ? C20 N4 C21 C22 7.1(6) . . . . ? Ag1 N4 C21 C22 -153.7(3) 1_545 . . . ? C20 O2 C22 C21 8.2(5) . . . . ? N4 C21 C22 O2 -9.1(6) . . . . ? O4 S1 C23 F2 60.8(7) . . . . ? O3 S1 C23 F2 -60.9(7) . . . . ? O5 S1 C23 F2 -179.8(6) . . . . ? O4 S1 C23 F1 -177.4(7) . . . . ? O3 S1 C23 F1 60.8(8) . . . . ? O5 S1 C23 F1 -58.0(8) . . . . ? O4 S1 C23 F3 -56.5(7) . . . . ? O3 S1 C23 F3 -178.3(6) . . . . ? O5 S1 C23 F3 62.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.105 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.117 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 765658' #TrackingRef '- NJ-ART-02-2010-000092R1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H64 Ag2 N14 O18' _chemical_formula_sum 'C48 H64 Ag2 N14 O18' _chemical_formula_weight 1340.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.5352(7) _cell_length_b 11.4453(14) _cell_length_c 22.023(3) _cell_angle_alpha 82.720(2) _cell_angle_beta 83.933(2) _cell_angle_gamma 87.015(2) _cell_volume 1375.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1968 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 21.24 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.798 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9245 _exptl_absorpt_correction_T_max 0.9612 _exptl_absorpt_process_details sadabs(Bruker,2001) _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 'Bruker Smart Apex CCD' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6872 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4769 _reflns_number_gt 3374 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart(Bruker,2001) _computing_cell_refinement Saintplus(Bruker,2001) _computing_data_reduction Saintplus(Bruker,2001) _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. The C-N bond lengths in the nitromethane molecules (N6-C23 and N7-C24) are shorter than expected. In the refinement process, the distances were fixed to reasonable values by the DFIX instruction. ; _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^)+(0.1520P)^2^+0.2866P] 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 4769 _refine_ls_number_parameters 364 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.2188 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.031 _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 1.81478(11) 0.15067(6) -0.38121(3) 0.0636(3) Uani 1 1 d . . . N1 N 1.7546(14) 0.3476(6) -0.3758(3) 0.068(2) Uani 1 1 d . . . N2 N 1.0795(10) 0.2766(4) -0.0735(2) 0.0371(12) Uani 1 1 d . . . H2A H 1.251(13) 0.244(6) -0.072(3) 0.044 Uiso 1 1 d . . . N3 N 0.8869(10) 0.2176(5) 0.0955(2) 0.0369(12) Uani 1 1 d . . . H3A H 0.737(13) 0.262(6) 0.095(3) 0.044 Uiso 1 1 d . . . N4 N 0.1006(11) 0.0446(6) 0.3717(3) 0.0550(15) Uani 1 1 d . . . N5 N 1.3444(13) 0.1946(6) -0.4508(4) 0.0644(18) Uani 1 1 d . . . N6 N 0.5961(11) -0.0321(5) 0.0761(3) 0.0518(15) Uani 1 1 d D . . N7 N 0.5980(12) 0.4731(5) 0.0819(3) 0.0530(15) Uani 1 1 d D . . O1 O 1.5405(18) 0.5208(5) -0.3748(3) 0.115(3) Uani 1 1 d . . . O2 O 0.0580(11) 0.2402(5) 0.3535(2) 0.0640(15) Uani 1 1 d . . . O3 O 1.3197(11) 0.1756(6) -0.3931(3) 0.0795(18) Uani 1 1 d . . . O4 O 1.1678(12) 0.2014(7) -0.4805(3) 0.089(2) Uani 1 1 d . . . O5 O 1.5538(13) 0.2018(8) -0.4767(3) 0.111(3) Uani 1 1 d . . . O6 O 0.5046(10) -0.1166(4) 0.0649(3) 0.0617(14) Uani 1 1 d . . . O7 O 0.8069(9) -0.0151(4) 0.0756(3) 0.0626(15) Uani 1 1 d . . . O8 O 0.8091(9) 0.4813(4) 0.0829(3) 0.0622(15) Uani 1 1 d . . . O9 O 0.4844(10) 0.3862(5) 0.0863(3) 0.0695(16) Uani 1 1 d . . . C1 C 1.715(3) 0.5394(9) -0.4295(5) 0.122(5) Uani 1 1 d . . . H1A H 1.8155 0.6056 -0.4276 0.147 Uiso 1 1 calc R . . H1B H 1.6332 0.5533 -0.4667 0.147 Uiso 1 1 calc R . . C2 C 1.867(2) 0.4244(9) -0.4274(4) 0.091(3) Uani 1 1 d . . . H2B H 1.8664 0.3899 -0.4654 0.109 Uiso 1 1 calc R . . H2C H 2.0343 0.4378 -0.4212 0.109 Uiso 1 1 calc R . . C3 C 1.5891(18) 0.4073(7) -0.3498(4) 0.066(2) Uani 1 1 d . . . C4 C 1.4237(15) 0.3710(6) -0.2934(3) 0.0556(19) Uani 1 1 d . . . C5 C 1.2215(17) 0.4385(7) -0.2771(4) 0.067(2) Uani 1 1 d . . . H5A H 1.1851 0.5080 -0.3017 0.081 Uiso 1 1 calc R . . C6 C 1.0695(17) 0.4039(7) -0.2238(3) 0.063(2) Uani 1 1 d . . . H6A H 0.9332 0.4505 -0.2128 0.076 Uiso 1 1 calc R . . C7 C 1.1228(13) 0.3001(6) -0.1876(3) 0.0439(16) Uani 1 1 d . . . C8 C 1.3265(15) 0.2321(8) -0.2050(3) 0.062(2) Uani 1 1 d . . . H8A H 1.3613 0.1619 -0.1808 0.074 Uiso 1 1 calc R . . C9 C 1.4788(16) 0.2655(8) -0.2569(4) 0.064(2) Uani 1 1 d . . . H9A H 1.6156 0.2190 -0.2677 0.077 Uiso 1 1 calc R . . C10 C 0.9591(13) 0.2627(7) -0.1304(3) 0.0471(17) Uani 1 1 d . . . H10A H 0.9196 0.1809 -0.1297 0.057 Uiso 1 1 calc R . . H10B H 0.8087 0.3101 -0.1306 0.057 Uiso 1 1 calc R . . C11 C 0.9165(11) 0.2454(6) -0.0155(3) 0.0386(14) Uani 1 1 d . . . H11A H 0.8526 0.1680 -0.0155 0.046 Uiso 1 1 calc R . . H11B H 0.7806 0.3022 -0.0131 0.046 Uiso 1 1 calc R . . C12 C 1.0611(11) 0.2455(6) 0.0393(3) 0.0368(14) Uani 1 1 d . . . H12A H 1.1934 0.1866 0.0381 0.044 Uiso 1 1 calc R . . H12B H 1.1285 0.3221 0.0391 0.044 Uiso 1 1 calc R . . C13 C 0.9930(12) 0.2130(7) 0.1558(3) 0.0464(16) Uani 1 1 d . . . H13A H 1.1162 0.1498 0.1594 0.056 Uiso 1 1 calc R . . H13B H 1.0683 0.2867 0.1582 0.056 Uiso 1 1 calc R . . C14 C 0.7919(13) 0.1923(6) 0.2065(3) 0.0459(16) Uani 1 1 d . . . C15 C 0.7478(15) 0.0806(7) 0.2367(4) 0.0582(19) Uani 1 1 d . . . H15A H 0.8514 0.0176 0.2270 0.070 Uiso 1 1 calc R . . C16 C 0.5542(14) 0.0610(7) 0.2807(3) 0.0566(19) Uani 1 1 d . . . H16A H 0.5295 -0.0146 0.3008 0.068 Uiso 1 1 calc R . . C17 C 0.3931(13) 0.1547(7) 0.2956(3) 0.0490(17) Uani 1 1 d . . . C18 C 0.4418(15) 0.2681(7) 0.2669(3) 0.0565(19) Uani 1 1 d . . . H18A H 0.3423 0.3320 0.2774 0.068 Uiso 1 1 calc R . . C19 C 0.6381(15) 0.2853(7) 0.2229(3) 0.0533(18) Uani 1 1 d . . . H19A H 0.6679 0.3612 0.2038 0.064 Uiso 1 1 calc R . . C20 C 0.1821(13) 0.1387(7) 0.3421(3) 0.0495(17) Uani 1 1 d . . . C21 C -0.1148(16) 0.0764(8) 0.4130(4) 0.068(2) Uani 1 1 d . . . H21A H -0.0895 0.0517 0.4557 0.081 Uiso 1 1 calc R . . H21B H -0.2587 0.0401 0.4036 0.081 Uiso 1 1 calc R . . C22 C -0.1396(15) 0.2096(8) 0.4003(4) 0.063(2) Uani 1 1 d . . . H22A H -0.2954 0.2343 0.3855 0.075 Uiso 1 1 calc R . . H22B H -0.1236 0.2459 0.4371 0.075 Uiso 1 1 calc R . . C23 C 0.4378(12) 0.0641(5) 0.0967(3) 0.048 Uani 1 1 d D . . C24 C 0.4622(12) 0.5858(5) 0.0737(3) 0.050 Uani 1 1 d 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 0.0569(5) 0.0713(5) 0.0571(5) 0.0018(3) 0.0106(3) -0.0079(3) N1 0.076(5) 0.076(5) 0.050(4) -0.008(3) 0.022(3) -0.029(4) N2 0.040(3) 0.036(3) 0.033(3) -0.001(2) 0.007(2) -0.003(2) N3 0.036(3) 0.039(3) 0.035(3) -0.004(2) 0.000(2) -0.001(2) N4 0.051(4) 0.070(4) 0.043(3) -0.007(3) 0.000(3) -0.004(3) N5 0.051(4) 0.072(5) 0.067(5) 0.003(4) -0.004(4) -0.012(3) N6 0.054(4) 0.053(4) 0.046(4) 0.008(3) -0.011(3) 0.002(3) N7 0.055(4) 0.059(4) 0.046(4) -0.010(3) -0.004(3) -0.001(3) O1 0.193(9) 0.055(4) 0.080(5) 0.001(3) 0.070(5) -0.025(5) O2 0.073(4) 0.063(3) 0.049(3) -0.002(3) 0.018(3) -0.002(3) O3 0.070(4) 0.106(5) 0.060(4) 0.002(3) 0.001(3) -0.028(4) O4 0.064(4) 0.112(5) 0.086(5) 0.013(4) -0.016(4) -0.015(4) O5 0.062(4) 0.192(9) 0.071(4) -0.003(5) 0.023(3) -0.024(5) O6 0.052(3) 0.046(3) 0.091(4) -0.012(3) -0.013(3) -0.016(2) O7 0.036(3) 0.039(3) 0.113(5) -0.008(3) -0.005(3) -0.006(2) O8 0.039(3) 0.037(3) 0.109(5) -0.004(3) -0.006(3) -0.003(2) O9 0.058(3) 0.053(3) 0.101(5) -0.010(3) -0.011(3) -0.018(3) C1 0.194(14) 0.074(7) 0.080(7) 0.000(6) 0.077(8) -0.032(8) C2 0.116(9) 0.088(7) 0.062(6) -0.002(5) 0.037(6) -0.044(6) C3 0.094(7) 0.055(5) 0.045(4) -0.006(4) 0.015(4) -0.023(5) C4 0.071(5) 0.050(4) 0.045(4) -0.006(3) 0.010(4) -0.019(4) C5 0.095(7) 0.048(4) 0.050(5) 0.011(4) 0.015(4) -0.001(4) C6 0.081(6) 0.057(5) 0.047(4) 0.001(4) 0.006(4) 0.007(4) C7 0.050(4) 0.046(4) 0.035(3) -0.005(3) 0.003(3) -0.007(3) C8 0.070(5) 0.068(5) 0.039(4) 0.010(4) 0.012(4) 0.004(4) C9 0.066(5) 0.076(5) 0.044(4) -0.001(4) 0.018(4) 0.001(4) C10 0.042(4) 0.062(4) 0.036(4) -0.004(3) 0.002(3) -0.010(3) C11 0.034(3) 0.048(4) 0.032(3) -0.002(3) 0.005(3) -0.004(3) C12 0.033(3) 0.040(3) 0.036(3) -0.004(3) 0.006(3) -0.003(3) C13 0.040(4) 0.060(4) 0.038(4) -0.004(3) -0.002(3) -0.005(3) C14 0.046(4) 0.058(4) 0.033(3) -0.006(3) -0.002(3) -0.006(3) C15 0.055(5) 0.064(5) 0.052(4) 0.000(4) 0.003(4) -0.001(4) C16 0.059(5) 0.056(4) 0.050(4) 0.008(3) 0.003(4) -0.007(4) C17 0.053(4) 0.065(5) 0.029(3) -0.001(3) -0.002(3) -0.011(4) C18 0.069(5) 0.054(4) 0.042(4) -0.006(3) 0.011(4) 0.001(4) C19 0.065(5) 0.054(4) 0.038(4) -0.004(3) 0.008(3) -0.006(4) C20 0.050(4) 0.066(5) 0.032(4) -0.005(3) -0.004(3) -0.007(4) C21 0.059(5) 0.089(6) 0.050(5) 0.000(4) 0.012(4) -0.001(4) C22 0.053(5) 0.083(6) 0.050(4) -0.009(4) 0.011(4) -0.011(4) C23 0.049 0.045 0.048 0.003 -0.008 0.007 C24 0.052 0.045 0.053 -0.007 -0.006 0.002 _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 2.247(7) 2_755 ? Ag1 N1 2.278(7) . ? N1 C3 1.247(11) . ? N1 C2 1.451(10) . ? N2 C11 1.499(8) . ? N2 C10 1.510(8) . ? N2 H2A 1.00(7) . ? N3 C13 1.502(9) . ? N3 C12 1.497(8) . ? N3 H3A 0.95(7) . ? N4 C20 1.265(9) . ? N4 C21 1.480(10) . ? N4 Ag1 2.247(7) 2_755 ? N5 O4 1.226(9) . ? N5 O5 1.239(9) . ? N5 O3 1.255(9) . ? N6 O6 1.180(7) . ? N6 O7 1.191(7) . ? N6 C23 1.458(2) . ? N7 O8 1.180(8) . ? N7 O9 1.192(8) . ? N7 C24 1.459(2) . ? O1 C3 1.371(11) . ? O1 C1 1.464(11) . ? O2 C20 1.356(9) . ? O2 C22 1.446(9) . ? C1 C2 1.523(17) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C4 1.490(10) . ? C4 C5 1.369(12) . ? C4 C9 1.401(11) . ? C5 C6 1.396(11) . ? C5 H5A 0.9300 . ? C6 C7 1.382(10) . ? C6 H6A 0.9300 . ? C7 C8 1.384(10) . ? C7 C10 1.501(9) . ? C8 C9 1.373(10) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.517(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.497(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.388(10) . ? C14 C15 1.385(10) . ? C15 C16 1.375(11) . ? C15 H15A 0.9300 . ? C16 C17 1.407(11) . ? C16 H16A 0.9300 . ? C17 C18 1.397(10) . ? C17 C20 1.472(10) . ? C18 C19 1.382(10) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C22 1.517(13) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? 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 170.6(2) 2_755 . ? C3 N1 C2 107.0(8) . . ? C3 N1 Ag1 132.9(5) . . ? C2 N1 Ag1 115.7(6) . . ? C11 N2 C10 112.4(5) . . ? C11 N2 H2A 114(4) . . ? C10 N2 H2A 117(4) . . ? C13 N3 C12 115.4(5) . . ? C13 N3 H3A 112(4) . . ? C12 N3 H3A 114(4) . . ? C20 N4 C21 108.0(7) . . ? C20 N4 Ag1 139.7(5) . 2_755 ? C21 N4 Ag1 112.3(5) . 2_755 ? O4 N5 O5 121.2(8) . . ? O4 N5 O3 121.1(7) . . ? O5 N5 O3 117.7(8) . . ? O6 N6 O7 128.5(6) . . ? O6 N6 C23 118.1(6) . . ? O7 N6 C23 113.4(6) . . ? O8 N7 O9 128.8(6) . . ? O8 N7 C24 114.3(6) . . ? O9 N7 C24 116.9(6) . . ? C3 O1 C1 104.6(8) . . ? C20 O2 C22 107.5(6) . . ? O1 C1 C2 103.5(8) . . ? O1 C1 H1A 111.1 . . ? C2 C1 H1A 111.1 . . ? O1 C1 H1B 111.1 . . ? C2 C1 H1B 111.1 . . ? H1A C1 H1B 109.0 . . ? N1 C2 C1 105.5(8) . . ? N1 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? N1 C2 H2C 110.6 . . ? C1 C2 H2C 110.6 . . ? H2B C2 H2C 108.8 . . ? N1 C3 O1 119.0(7) . . ? N1 C3 C4 128.4(8) . . ? O1 C3 C4 112.5(8) . . ? C5 C4 C9 120.1(7) . . ? C5 C4 C3 121.3(7) . . ? C9 C4 C3 118.6(8) . . ? C4 C5 C6 120.6(7) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C7 C6 C5 119.6(8) . . ? C7 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? C8 C7 C6 119.1(7) . . ? C8 C7 C10 121.2(6) . . ? C6 C7 C10 119.7(7) . . ? C9 C8 C7 121.9(7) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C8 C9 C4 118.6(8) . . ? C8 C9 H9A 120.7 . . ? C4 C9 H9A 120.7 . . ? C7 C10 N2 111.0(5) . . ? C7 C10 H10A 109.4 . . ? N2 C10 H10A 109.4 . . ? C7 C10 H10B 109.4 . . ? N2 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C12 109.0(5) . . ? N2 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N2 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N3 C12 C11 106.4(5) . . ? N3 C12 H12A 110.5 . . ? C11 C12 H12A 110.5 . . ? N3 C12 H12B 110.5 . . ? C11 C12 H12B 110.5 . . ? H12A C12 H12B 108.6 . . ? C14 C13 N3 108.2(5) . . ? C14 C13 H13A 110.0 . . ? N3 C13 H13A 110.0 . . ? C14 C13 H13B 110.0 . . ? N3 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? C19 C14 C15 118.1(7) . . ? C19 C14 C13 120.2(6) . . ? C15 C14 C13 121.6(7) . . ? C16 C15 C14 121.4(8) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C15 C16 C17 120.3(7) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C18 C17 C16 118.5(7) . . ? C18 C17 C20 118.8(7) . . ? C16 C17 C20 122.7(7) . . ? C19 C18 C17 119.9(7) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C14 121.7(7) . . ? C18 C19 H19A 119.2 . . ? C14 C19 H19A 119.2 . . ? N4 C20 O2 116.5(7) . . ? N4 C20 C17 129.2(7) . . ? O2 C20 C17 114.4(7) . . ? N4 C21 C22 104.2(6) . . ? N4 C21 H21A 110.9 . . ? C22 C21 H21A 110.9 . . ? N4 C21 H21B 110.9 . . ? C22 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? O2 C22 C21 103.9(6) . . ? O2 C22 H22A 111.0 . . ? C21 C22 H22A 111.0 . . ? O2 C22 H22B 111.0 . . ? C21 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? 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 C3 O1 C1 C2 -3.0(13) . . . . ? C3 N1 C2 C1 -5.3(12) . . . . ? Ag1 N1 C2 C1 154.3(8) . . . . ? O1 C1 C2 N1 4.9(13) . . . . ? C2 N1 C3 O1 3.7(12) . . . . ? Ag1 N1 C3 O1 -150.9(7) . . . . ? C2 N1 C3 C4 -177.9(9) . . . . ? Ag1 N1 C3 C4 27.5(15) . . . . ? C1 O1 C3 N1 -0.4(14) . . . . ? C1 O1 C3 C4 -178.9(9) . . . . ? N1 C3 C4 C5 -167.3(9) . . . . ? O1 C3 C4 C5 11.1(12) . . . . ? N1 C3 C4 C9 12.7(14) . . . . ? O1 C3 C4 C9 -168.9(8) . . . . ? C9 C4 C5 C6 0.6(13) . . . . ? C3 C4 C5 C6 -179.4(8) . . . . ? C4 C5 C6 C7 -0.6(13) . . . . ? C5 C6 C7 C8 -0.1(12) . . . . ? C5 C6 C7 C10 -179.9(7) . . . . ? C6 C7 C8 C9 0.6(13) . . . . ? C10 C7 C8 C9 -179.6(7) . . . . ? C7 C8 C9 C4 -0.5(13) . . . . ? C5 C4 C9 C8 -0.1(13) . . . . ? C3 C4 C9 C8 179.9(8) . . . . ? C8 C7 C10 N2 72.2(9) . . . . ? C6 C7 C10 N2 -108.0(8) . . . . ? C11 N2 C10 C7 177.3(6) . . . . ? C10 N2 C11 C12 172.4(5) . . . . ? C13 N3 C12 C11 179.9(5) . . . . ? N2 C11 C12 N3 178.2(5) . . . . ? C12 N3 C13 C14 176.3(5) . . . . ? N3 C13 C14 C19 -80.3(8) . . . . ? N3 C13 C14 C15 97.4(8) . . . . ? C19 C14 C15 C16 1.6(11) . . . . ? C13 C14 C15 C16 -176.1(7) . . . . ? C14 C15 C16 C17 0.8(12) . . . . ? C15 C16 C17 C18 -3.1(12) . . . . ? C15 C16 C17 C20 179.7(7) . . . . ? C16 C17 C18 C19 3.0(11) . . . . ? C20 C17 C18 C19 -179.7(7) . . . . ? C17 C18 C19 C14 -0.6(12) . . . . ? C15 C14 C19 C18 -1.7(11) . . . . ? C13 C14 C19 C18 176.0(7) . . . . ? C21 N4 C20 O2 -1.2(9) . . . . ? Ag1 N4 C20 O2 180.0(5) 2_755 . . . ? C21 N4 C20 C17 179.8(7) . . . . ? Ag1 N4 C20 C17 1.0(13) 2_755 . . . ? C22 O2 C20 N4 1.6(9) . . . . ? C22 O2 C20 C17 -179.2(6) . . . . ? C18 C17 C20 N4 177.2(8) . . . . ? C16 C17 C20 N4 -5.6(12) . . . . ? C18 C17 C20 O2 -1.8(10) . . . . ? C16 C17 C20 O2 175.4(7) . . . . ? C20 N4 C21 C22 0.2(9) . . . . ? Ag1 N4 C21 C22 179.4(5) 2_755 . . . ? C20 O2 C22 C21 -1.3(8) . . . . ? N4 C21 C22 O2 0.6(9) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.750 _refine_diff_density_min -1.100 _refine_diff_density_rms 0.136 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 765659' #TrackingRef '- NJ-ART-02-2010-000092R1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H56 Ag2 N10 O11' _chemical_formula_sum 'C45 H56 Ag2 N10 O11' _chemical_formula_weight 1128.74 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' _symmetry_space_group_name_HALL '-C 2yc' 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 14.0161(8) _cell_length_b 8.7983(5) _cell_length_c 40.648(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.3990(10) _cell_angle_gamma 90.00 _cell_volume 4958.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4229 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 23.2 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_T_max 0.9665 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'Bruker Smart Apex CCd' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12014 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4359 _reflns_number_gt 3970 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _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. The nitrate anions are disordered. In the refinement process, the geometry was deformed and the thermal factors became unreasonable. Thus the geometry of the anions was restrained by the DFIX, SADI instructions for N-O and O-O distances. In addition, the whole nitrate anion was restrained by FLAT instruction for its planarity. The thermal factors of the oxygen atoms in the anions were restrained using ISOR instruction. ; _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^)+(0.0586P)^2^+30.2858P] 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 4359 _refine_ls_number_parameters 331 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.1695 _refine_ls_wR_factor_gt 0.1654 _refine_ls_goodness_of_fit_ref 1.222 _refine_ls_restrained_S_all 1.226 _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 0.25293(4) -0.08050(6) 0.137217(12) 0.0486(2) Uani 1 1 d . . . O1 O 0.5265(4) 0.4468(6) 0.04965(12) 0.0668(14) Uani 1 1 d . . . O2 O -0.0434(4) -0.7269(6) 0.07029(12) 0.0633(13) Uani 1 1 d . . . N1 N 0.3092(4) 0.0993(5) 0.17974(13) 0.0455(12) Uani 1 1 d . . . H1A H 0.3729 0.0810 0.1865 0.055 Uiso 1 1 calc R . . N2 N 0.2031(4) -0.1934(5) 0.18577(12) 0.0426(12) Uani 1 1 d . . . H2A H 0.1397 -0.1712 0.1858 0.051 Uiso 1 1 calc R . . N3 N 0.6447(4) 0.5042(7) 0.09089(13) 0.0526(14) Uani 1 1 d . . . N4 N -0.1544(4) -0.7122(6) 0.10420(13) 0.0489(13) Uani 1 1 d . . . C1 C 0.2573(6) 0.0582(8) 0.20676(18) 0.0583(19) Uani 1 1 d . . . H1B H 0.1908 0.0909 0.2014 0.070 Uiso 1 1 calc R . . H1C H 0.2855 0.1112 0.2268 0.070 Uiso 1 1 calc R . . C2 C 0.2598(6) -0.1107(8) 0.21334(16) 0.0567(18) Uani 1 1 d . . . H2B H 0.3261 -0.1460 0.2161 0.068 Uiso 1 1 calc R . . H2C H 0.2341 -0.1312 0.2338 0.068 Uiso 1 1 calc R . . C3 C 0.2982(5) 0.2613(7) 0.17138(19) 0.0577(18) Uani 1 1 d . . . H3B H 0.3102 0.3208 0.1916 0.069 Uiso 1 1 calc R . . H3C H 0.2324 0.2804 0.1611 0.069 Uiso 1 1 calc R . . C4 C 0.2156(5) -0.3583(7) 0.18968(17) 0.0538(17) Uani 1 1 d . . . H4B H 0.2095 -0.3866 0.2123 0.065 Uiso 1 1 calc R . . H4C H 0.2798 -0.3862 0.1856 0.065 Uiso 1 1 calc R . . C5 C 0.3663(5) 0.3119(7) 0.14803(17) 0.0462(15) Uani 1 1 d . . . C6 C 0.3557(6) 0.2621(8) 0.11534(19) 0.064(2) Uani 1 1 d . . . H6A H 0.3046 0.1977 0.1077 0.077 Uiso 1 1 calc R . . C7 C 0.4173(6) 0.3043(8) 0.09408(18) 0.0608(19) Uani 1 1 d . . . H7A H 0.4090 0.2671 0.0724 0.073 Uiso 1 1 calc R . . C8 C 0.4925(5) 0.4028(7) 0.10483(16) 0.0450(15) Uani 1 1 d . . . C9 C 0.5028(5) 0.4564(7) 0.13708(17) 0.0473(15) Uani 1 1 d . . . H9A H 0.5522 0.5243 0.1444 0.057 Uiso 1 1 calc R . . C10 C 0.4405(5) 0.4104(8) 0.15872(18) 0.0539(17) Uani 1 1 d . . . H10A H 0.4489 0.4463 0.1805 0.065 Uiso 1 1 calc R . . C11 C 0.5598(5) 0.4539(7) 0.08272(16) 0.0478(15) Uani 1 1 d . . . C12 C 0.6787(6) 0.5538(10) 0.05993(18) 0.067(2) Uani 1 1 d . . . H12A H 0.7419 0.5119 0.0584 0.081 Uiso 1 1 calc R . . H12B H 0.6824 0.6638 0.0590 0.081 Uiso 1 1 calc R . . C13 C 0.6052(7) 0.4943(14) 0.03250(19) 0.086(3) Uani 1 1 d . . . H13A H 0.5845 0.5731 0.0163 0.103 Uiso 1 1 calc R . . H13B H 0.6305 0.4093 0.0213 0.103 Uiso 1 1 calc R . . C14 C 0.1418(5) -0.4437(6) 0.16598(17) 0.0445(15) Uani 1 1 d . . . C15 C 0.0699(5) -0.5279(7) 0.17758(16) 0.0473(15) Uani 1 1 d . . . H15A H 0.0671 -0.5314 0.2003 0.057 Uiso 1 1 calc R . . C16 C 0.0035(5) -0.6052(7) 0.15627(16) 0.0475(15) Uani 1 1 d . . . H16A H -0.0441 -0.6606 0.1646 0.057 Uiso 1 1 calc R . . C17 C 0.0055(5) -0.6030(7) 0.12231(16) 0.0429(14) Uani 1 1 d . . . C18 C 0.0779(5) -0.5211(8) 0.11042(17) 0.0542(17) Uani 1 1 d . . . H18A H 0.0811 -0.5184 0.0877 0.065 Uiso 1 1 calc R . . C19 C 0.1449(5) -0.4437(7) 0.13238(18) 0.0535(17) Uani 1 1 d . . . H19A H 0.1936 -0.3900 0.1242 0.064 Uiso 1 1 calc R . . C20 C -0.0689(5) -0.6826(7) 0.09927(15) 0.0443(14) Uani 1 1 d . . . C21 C -0.1993(6) -0.8048(9) 0.07581(18) 0.0620(19) Uani 1 1 d . . . H21A H -0.2633 -0.7679 0.0673 0.074 Uiso 1 1 calc R . . H21B H -0.2035 -0.9108 0.0820 0.074 Uiso 1 1 calc R . . C22 C -0.1310(6) -0.7841(10) 0.05066(19) 0.070(2) Uani 1 1 d . . . H22A H -0.1193 -0.8799 0.0401 0.084 Uiso 1 1 calc R . . H22B H -0.1566 -0.7116 0.0336 0.084 Uiso 1 1 calc R . . N5 N 0.5000 0.2106(12) 0.2500 0.068(3) Uani 1 2 d S . . O3 O 0.5000 0.0742(12) 0.2500 0.132(5) Uani 1 2 d S . . O4 O 0.5611(8) 0.2876(11) 0.2405(3) 0.167(4) Uani 1 1 d . . . C23 C 0.4301(14) -0.417(2) 0.2443(8) 0.115(9) Uani 0.50 1 d P . . O5 O 0.5000 -0.331(2) 0.2500 0.196(7) Uani 1 2 d S . . N6 N 0.816(2) 0.591(3) -0.0074(5) 0.24(3) Uani 0.50 1 d PD . . O6 O 0.7378(17) 0.642(3) -0.0178(6) 0.27(2) Uani 0.50 1 d PDU . . O7 O 0.867(2) 0.659(3) 0.0136(6) 0.255(18) Uani 0.50 1 d PDU . . O8 O 0.841(3) 0.469(3) -0.0164(6) 0.35(3) Uani 0.50 1 d PDU . . 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 0.0543(3) 0.0528(3) 0.0397(3) -0.0041(2) 0.0097(2) -0.0070(2) O1 0.062(3) 0.091(4) 0.045(3) 0.002(3) -0.002(2) -0.021(3) O2 0.063(3) 0.079(4) 0.052(3) -0.023(3) 0.023(2) -0.009(3) N1 0.053(3) 0.035(3) 0.050(3) -0.001(2) 0.013(2) 0.000(2) N2 0.049(3) 0.037(3) 0.042(3) 0.001(2) 0.007(2) -0.003(2) N3 0.048(3) 0.062(4) 0.046(3) 0.010(3) 0.004(3) -0.009(3) N4 0.046(3) 0.051(3) 0.050(3) -0.010(3) 0.010(2) 0.001(3) C1 0.081(5) 0.046(4) 0.052(4) -0.012(3) 0.024(4) -0.014(4) C2 0.083(5) 0.049(4) 0.039(3) 0.000(3) 0.013(3) -0.008(4) C3 0.060(4) 0.040(4) 0.077(5) -0.001(3) 0.026(4) 0.006(3) C4 0.066(5) 0.039(3) 0.053(4) 0.008(3) -0.002(3) 0.002(3) C5 0.046(4) 0.032(3) 0.063(4) 0.002(3) 0.016(3) -0.002(3) C6 0.066(5) 0.056(4) 0.068(5) -0.002(4) 0.004(4) -0.031(4) C7 0.069(5) 0.058(4) 0.054(4) -0.001(3) 0.004(4) -0.023(4) C8 0.045(4) 0.040(3) 0.049(4) 0.008(3) 0.002(3) 0.006(3) C9 0.039(3) 0.040(3) 0.063(4) -0.006(3) 0.007(3) -0.003(3) C10 0.058(4) 0.049(4) 0.056(4) -0.010(3) 0.014(3) 0.012(3) C11 0.050(4) 0.043(4) 0.048(4) 0.001(3) -0.001(3) -0.002(3) C12 0.068(5) 0.082(6) 0.051(4) 0.016(4) 0.006(4) -0.015(4) C13 0.078(6) 0.142(9) 0.038(4) 0.007(5) 0.008(4) -0.032(6) C14 0.051(4) 0.028(3) 0.055(4) 0.004(3) 0.009(3) 0.007(3) C15 0.051(4) 0.049(4) 0.044(4) 0.005(3) 0.014(3) 0.008(3) C16 0.048(4) 0.047(4) 0.051(4) -0.001(3) 0.020(3) -0.002(3) C17 0.046(4) 0.035(3) 0.050(4) -0.002(3) 0.016(3) 0.008(3) C18 0.069(5) 0.050(4) 0.047(4) -0.003(3) 0.019(3) -0.009(3) C19 0.061(4) 0.043(4) 0.058(4) 0.005(3) 0.017(3) -0.011(3) C20 0.053(4) 0.037(3) 0.044(3) -0.002(3) 0.013(3) 0.005(3) C21 0.059(5) 0.069(5) 0.058(4) -0.016(4) 0.008(3) -0.006(4) C22 0.070(5) 0.085(6) 0.056(4) -0.016(4) 0.011(4) -0.008(4) N5 0.087(7) 0.065(6) 0.060(5) 0.000 0.043(5) 0.000 O3 0.229(15) 0.072(7) 0.117(9) 0.000 0.095(10) 0.000 O4 0.168(9) 0.118(7) 0.244(12) 0.042(7) 0.127(9) 0.013(6) C23 0.053(11) 0.075(13) 0.20(3) 0.007(15) -0.022(14) -0.010(10) O5 0.167(16) 0.162(15) 0.25(2) 0.000 -0.016(14) 0.000 N6 0.43(8) 0.18(4) 0.09(2) 0.06(2) -0.06(3) -0.16(5) O6 0.29(4) 0.37(5) 0.14(2) 0.09(3) -0.05(2) -0.22(4) O7 0.36(4) 0.31(4) 0.098(16) -0.05(2) 0.02(2) -0.15(4) O8 0.61(7) 0.21(3) 0.15(2) 0.08(2) -0.18(3) -0.21(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 Ag1 N4 2.311(5) 3 ? Ag1 N3 2.360(5) 3_445 ? Ag1 N1 2.390(5) . ? Ag1 N2 2.403(5) . ? O1 C11 1.358(8) . ? O1 C13 1.449(9) . ? O2 C20 1.338(7) . ? O2 C22 1.454(9) . ? N1 C1 1.448(8) . ? N1 C3 1.468(8) . ? N1 H1A 0.9100 . ? N2 C4 1.467(8) . ? N2 C2 1.469(8) . ? N2 H2A 0.9100 . ? N3 C11 1.267(8) . ? N3 C12 1.475(9) . ? N3 Ag1 2.360(5) 3 ? N4 C20 1.270(8) . ? N4 C21 1.476(9) . ? N4 Ag1 2.311(5) 3_445 ? C1 C2 1.510(9) . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 C5 1.508(9) . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 C14 1.507(10) . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 C10 1.374(9) . ? C5 C6 1.386(10) . ? C6 C7 1.360(10) . ? C6 H6A 0.9300 . ? C7 C8 1.385(9) . ? C7 H7A 0.9300 . ? C8 C9 1.381(9) . ? C8 C11 1.466(9) . ? C9 C10 1.387(10) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? C12 C13 1.498(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C19 1.373(9) . ? C14 C15 1.388(9) . ? C15 C16 1.357(10) . ? C15 H15A 0.9300 . ? C16 C17 1.385(9) . ? C16 H16A 0.9300 . ? C17 C18 1.388(9) . ? C17 C20 1.473(9) . ? C18 C19 1.378(10) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C22 1.510(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? N5 O4 1.199(10) . ? N5 O4 1.199(10) 2_655 ? N5 O3 1.201(12) . ? C23 O5 1.24(2) . ? O5 C23 1.24(2) 2_655 ? N6 O7 1.197(18) . ? N6 O8 1.199(19) . ? N6 O6 1.202(19) . ? 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 N3 92.6(2) 3 3_445 ? N4 Ag1 N1 126.73(19) 3 . ? N3 Ag1 N1 118.28(19) 3_445 . ? N4 Ag1 N2 121.69(19) 3 . ? N3 Ag1 N2 123.77(18) 3_445 . ? N1 Ag1 N2 77.54(17) . . ? C11 O1 C13 106.7(5) . . ? C20 O2 C22 105.7(5) . . ? C1 N1 C3 111.8(5) . . ? C1 N1 Ag1 103.6(4) . . ? C3 N1 Ag1 117.6(4) . . ? C1 N1 H1A 107.8 . . ? C3 N1 H1A 107.8 . . ? Ag1 N1 H1A 107.8 . . ? C4 N2 C2 111.4(5) . . ? C4 N2 Ag1 116.9(4) . . ? C2 N2 Ag1 103.4(4) . . ? C4 N2 H2A 108.3 . . ? C2 N2 H2A 108.3 . . ? Ag1 N2 H2A 108.3 . . ? C11 N3 C12 106.7(6) . . ? C11 N3 Ag1 124.6(5) . 3 ? C12 N3 Ag1 121.6(5) . 3 ? C20 N4 C21 107.1(5) . . ? C20 N4 Ag1 127.7(4) . 3_445 ? C21 N4 Ag1 121.3(4) . 3_445 ? N1 C1 C2 112.2(6) . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? N1 C1 H1C 109.2 . . ? C2 C1 H1C 109.2 . . ? H1B C1 H1C 107.9 . . ? N2 C2 C1 110.9(6) . . ? N2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? C1 C2 H2C 109.5 . . ? H2B C2 H2C 108.1 . . ? N1 C3 C5 112.2(5) . . ? N1 C3 H3B 109.2 . . ? C5 C3 H3B 109.2 . . ? N1 C3 H3C 109.2 . . ? C5 C3 H3C 109.2 . . ? H3B C3 H3C 107.9 . . ? N2 C4 C14 111.3(5) . . ? N2 C4 H4B 109.4 . . ? C14 C4 H4B 109.4 . . ? N2 C4 H4C 109.4 . . ? C14 C4 H4C 109.4 . . ? H4B C4 H4C 108.0 . . ? C10 C5 C6 118.2(6) . . ? C10 C5 C3 120.4(6) . . ? C6 C5 C3 121.3(6) . . ? C7 C6 C5 122.2(6) . . ? C7 C6 H6A 118.9 . . ? C5 C6 H6A 118.9 . . ? C6 C7 C8 119.7(7) . . ? C6 C7 H7A 120.2 . . ? C8 C7 H7A 120.2 . . ? C9 C8 C7 118.8(6) . . ? C9 C8 C11 119.3(6) . . ? C7 C8 C11 121.8(6) . . ? C8 C9 C10 121.0(6) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C5 C10 C9 120.0(6) . . ? C5 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? N3 C11 O1 116.7(6) . . ? N3 C11 C8 127.6(6) . . ? O1 C11 C8 115.7(6) . . ? N3 C12 C13 105.0(6) . . ? N3 C12 H12A 110.8 . . ? C13 C12 H12A 110.8 . . ? N3 C12 H12B 110.8 . . ? C13 C12 H12B 110.8 . . ? H12A C12 H12B 108.8 . . ? O1 C13 C12 103.4(6) . . ? O1 C13 H13A 111.1 . . ? C12 C13 H13A 111.1 . . ? O1 C13 H13B 111.1 . . ? C12 C13 H13B 111.1 . . ? H13A C13 H13B 109.0 . . ? C19 C14 C15 117.9(6) . . ? C19 C14 C4 121.2(6) . . ? C15 C14 C4 120.9(6) . . ? C16 C15 C14 121.0(6) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 121.2(6) . . ? C15 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? C16 C17 C18 118.5(6) . . ? C16 C17 C20 120.8(6) . . ? C18 C17 C20 120.7(6) . . ? C19 C18 C17 119.7(6) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C14 C19 C18 121.8(6) . . ? C14 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? N4 C20 O2 117.3(6) . . ? N4 C20 C17 126.4(6) . . ? O2 C20 C17 116.3(6) . . ? N4 C21 C22 102.9(6) . . ? N4 C21 H21A 111.2 . . ? C22 C21 H21A 111.2 . . ? N4 C21 H21B 111.2 . . ? C22 C21 H21B 111.2 . . ? H21A C21 H21B 109.1 . . ? O2 C22 C21 103.8(6) . . ? O2 C22 H22A 111.0 . . ? C21 C22 H22A 111.0 . . ? O2 C22 H22B 111.0 . . ? C21 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? O4 N5 O4 111.2(12) . 2_655 ? O4 N5 O3 124.4(6) . . ? O4 N5 O3 124.4(6) 2_655 . ? C23 O5 C23 104(2) . 2_655 ? O7 N6 O8 119.6(17) . . ? O7 N6 O6 118.8(17) . . ? O8 N6 O6 121.5(17) . . ? 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 N4 Ag1 N1 C1 -136.1(4) 3 . . . ? N3 Ag1 N1 C1 106.1(4) 3_445 . . . ? N2 Ag1 N1 C1 -15.7(4) . . . . ? N4 Ag1 N1 C3 100.1(5) 3 . . . ? N3 Ag1 N1 C3 -17.7(5) 3_445 . . . ? N2 Ag1 N1 C3 -139.5(5) . . . . ? N4 Ag1 N2 C4 -12.8(5) 3 . . . ? N3 Ag1 N2 C4 105.6(5) 3_445 . . . ? N1 Ag1 N2 C4 -138.5(5) . . . . ? N4 Ag1 N2 C2 109.9(4) 3 . . . ? N3 Ag1 N2 C2 -131.6(4) 3_445 . . . ? N1 Ag1 N2 C2 -15.8(4) . . . . ? C3 N1 C1 C2 174.4(6) . . . . ? Ag1 N1 C1 C2 46.8(7) . . . . ? C4 N2 C2 C1 172.3(6) . . . . ? Ag1 N2 C2 C1 45.9(6) . . . . ? N1 C1 C2 N2 -68.7(8) . . . . ? C1 N1 C3 C5 169.1(6) . . . . ? Ag1 N1 C3 C5 -71.3(7) . . . . ? C2 N2 C4 C14 167.5(6) . . . . ? Ag1 N2 C4 C14 -74.0(7) . . . . ? N1 C3 C5 C10 -112.0(7) . . . . ? N1 C3 C5 C6 68.6(9) . . . . ? C10 C5 C6 C7 1.8(11) . . . . ? C3 C5 C6 C7 -178.8(7) . . . . ? C5 C6 C7 C8 -1.4(12) . . . . ? C6 C7 C8 C9 -0.2(11) . . . . ? C6 C7 C8 C11 -178.8(7) . . . . ? C7 C8 C9 C10 1.4(10) . . . . ? C11 C8 C9 C10 -180.0(6) . . . . ? C6 C5 C10 C9 -0.6(10) . . . . ? C3 C5 C10 C9 180.0(6) . . . . ? C8 C9 C10 C5 -1.0(10) . . . . ? C12 N3 C11 O1 5.0(9) . . . . ? Ag1 N3 C11 O1 -145.8(5) 3 . . . ? C12 N3 C11 C8 -174.7(7) . . . . ? Ag1 N3 C11 C8 34.5(10) 3 . . . ? C13 O1 C11 N3 3.2(9) . . . . ? C13 O1 C11 C8 -177.1(7) . . . . ? C9 C8 C11 N3 24.0(10) . . . . ? C7 C8 C11 N3 -157.4(7) . . . . ? C9 C8 C11 O1 -155.7(6) . . . . ? C7 C8 C11 O1 22.9(9) . . . . ? C11 N3 C12 C13 -10.7(9) . . . . ? Ag1 N3 C12 C13 141.1(6) 3 . . . ? C11 O1 C13 C12 -9.6(10) . . . . ? N3 C12 C13 O1 12.1(10) . . . . ? N2 C4 C14 C19 69.8(8) . . . . ? N2 C4 C14 C15 -111.8(7) . . . . ? C19 C14 C15 C16 -1.4(9) . . . . ? C4 C14 C15 C16 -179.8(6) . . . . ? C14 C15 C16 C17 0.2(10) . . . . ? C15 C16 C17 C18 0.8(10) . . . . ? C15 C16 C17 C20 -177.7(6) . . . . ? C16 C17 C18 C19 -0.5(10) . . . . ? C20 C17 C18 C19 178.0(6) . . . . ? C15 C14 C19 C18 1.6(10) . . . . ? C4 C14 C19 C18 -179.9(6) . . . . ? C17 C18 C19 C14 -0.7(11) . . . . ? C21 N4 C20 O2 5.4(8) . . . . ? Ag1 N4 C20 O2 -152.2(5) 3_445 . . . ? C21 N4 C20 C17 -175.0(6) . . . . ? Ag1 N4 C20 C17 27.4(9) 3_445 . . . ? C22 O2 C20 N4 6.6(8) . . . . ? C22 O2 C20 C17 -173.0(6) . . . . ? C16 C17 C20 N4 26.2(10) . . . . ? C18 C17 C20 N4 -152.3(7) . . . . ? C16 C17 C20 O2 -154.2(6) . . . . ? C18 C17 C20 O2 27.3(9) . . . . ? C20 N4 C21 C22 -14.4(8) . . . . ? Ag1 N4 C21 C22 145.0(5) 3_445 . . . ? C20 O2 C22 C21 -15.0(8) . . . . ? N4 C21 C22 O2 17.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.858 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.109 #====END data_5 _database_code_depnum_ccdc_archive 'CCDC 765660' #TrackingRef '- NJ-ART-02-2010-000092R1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 Ag B F4 N4 O2' _chemical_formula_sum 'C22 H26 Ag B F4 N4 O2' _chemical_formula_weight 573.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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' _symmetry_space_group_name_HALL '-C 2yc' 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 15.250(9) _cell_length_b 8.2253(5) _cell_length_c 39.011(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.4250(10) _cell_angle_gamma 90.00 _cell_volume 4813(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4078 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8555 _exptl_absorpt_correction_T_max 0.9318 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'Bruker Smart Apex CCd' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11524 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4240 _reflns_number_gt 3702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _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^)+(0.0785P)^2^+23.3804P] 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 4240 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1638 _refine_ls_wR_factor_gt 0.1578 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 0.79368(3) 0.05068(5) 0.379257(10) 0.0481(2) Uani 1 1 d . . . O1 O 0.5667(3) 0.7941(5) 0.31536(10) 0.0529(10) Uani 1 1 d . . . O2 O 0.8394(3) -0.6856(5) 0.28367(10) 0.0588(11) Uani 1 1 d . . . N1 N 0.6544(3) 0.9718(5) 0.34969(12) 0.0415(10) Uani 1 1 d . . . N2 N 0.8051(3) 0.2142(5) 0.43178(11) 0.0406(10) Uani 1 1 d . . . H2C H 0.8455 0.2945 0.4306 0.049 Uiso 1 1 calc R . . N3 N 0.8915(3) -0.1046(5) 0.42165(11) 0.0405(10) Uani 1 1 d . . . H3A H 0.8583 -0.1826 0.4298 0.049 Uiso 1 1 calc R . . N4 N 0.8374(3) -0.8644(6) 0.32701(12) 0.0493(12) Uani 1 1 d . . . C1 C 0.8444(4) 0.1021(7) 0.45984(14) 0.0502(14) Uani 1 1 d . . . H1A H 0.7992 0.0259 0.4643 0.060 Uiso 1 1 calc R . . H1B H 0.8647 0.1634 0.4810 0.060 Uiso 1 1 calc R . . C2 C 0.7234(4) 0.2907(8) 0.43898(16) 0.0533(15) Uani 1 1 d . . . H2A H 0.7336 0.3306 0.4628 0.064 Uiso 1 1 calc R . . H2B H 0.6761 0.2105 0.4366 0.064 Uiso 1 1 calc R . . C3 C 0.6953(4) 0.4300(7) 0.41419(15) 0.0441(13) Uani 1 1 d . . . C4 C 0.6965(4) 0.5891(7) 0.42644(15) 0.0464(13) Uani 1 1 d . . . H4A H 0.7132 0.6092 0.4502 0.056 Uiso 1 1 calc R . . C5 C 0.6736(4) 0.7156(7) 0.40413(14) 0.0467(13) Uani 1 1 d . . . H5A H 0.6757 0.8210 0.4128 0.056 Uiso 1 1 calc R . . C6 C 0.6475(3) 0.6899(6) 0.36876(13) 0.0388(12) Uani 1 1 d . . . C7 C 0.6440(4) 0.5306(7) 0.35623(15) 0.0478(14) Uani 1 1 d . . . H7A H 0.6248 0.5100 0.3326 0.057 Uiso 1 1 calc R . . C8 C 0.6688(4) 0.4048(7) 0.37893(15) 0.0508(14) Uani 1 1 d . . . H8A H 0.6678 0.2993 0.3703 0.061 Uiso 1 1 calc R . . C9 C 0.6253(3) 0.8268(7) 0.34486(13) 0.0395(12) Uani 1 1 d . . . C10 C 0.6056(4) 1.0688(7) 0.32034(15) 0.0513(14) Uani 1 1 d . . . H10A H 0.6463 1.1353 0.3099 0.062 Uiso 1 1 calc R . . H10B H 0.5616 1.1386 0.3280 0.062 Uiso 1 1 calc R . . C11 C 0.5612(4) 0.9414(7) 0.29488(15) 0.0535(15) Uani 1 1 d . . . H11A H 0.4996 0.9700 0.2859 0.064 Uiso 1 1 calc R . . H11B H 0.5924 0.9294 0.2755 0.064 Uiso 1 1 calc R . . C12 C 0.9212(4) 0.0101(7) 0.45023(15) 0.0492(14) Uani 1 1 d . . . H12A H 0.9633 0.0862 0.4433 0.059 Uiso 1 1 calc R . . H12B H 0.9516 -0.0491 0.4704 0.059 Uiso 1 1 calc R . . C13 C 0.9671(4) -0.1852(8) 0.41049(17) 0.0561(15) Uani 1 1 d . . . H13A H 1.0077 -0.2250 0.4308 0.067 Uiso 1 1 calc R . . H13B H 0.9990 -0.1071 0.3988 0.067 Uiso 1 1 calc R . . C14 C 0.9374(4) -0.3252(7) 0.38626(15) 0.0458(13) Uani 1 1 d . . . C15 C 0.9561(4) -0.4838(8) 0.39612(15) 0.0480(14) Uani 1 1 d . . . H15A H 0.9880 -0.5052 0.4183 0.058 Uiso 1 1 calc R . . C16 C 0.9291(4) -0.6108(7) 0.37411(14) 0.0458(13) Uani 1 1 d . . . H16A H 0.9436 -0.7167 0.3814 0.055 Uiso 1 1 calc R . . C17 C 0.8805(4) -0.5832(7) 0.34127(14) 0.0417(12) Uani 1 1 d . . . C18 C 0.8621(5) -0.4236(7) 0.33089(16) 0.0560(16) Uani 1 1 d . . . H18A H 0.8302 -0.4023 0.3087 0.067 Uiso 1 1 calc R . . C19 C 0.8902(5) -0.2985(8) 0.35271(17) 0.0608(17) Uani 1 1 d . . . H19A H 0.8777 -0.1924 0.3451 0.073 Uiso 1 1 calc R . . C20 C 0.8514(4) -0.7198(7) 0.31794(14) 0.0451(13) Uani 1 1 d . . . C21 C 0.8179(5) -0.9606(8) 0.29469(16) 0.0601(17) Uani 1 1 d . . . H21A H 0.7637 -1.0235 0.2938 0.072 Uiso 1 1 calc R . . H21B H 0.8666 -1.0340 0.2929 0.072 Uiso 1 1 calc R . . C22 C 0.8068(6) -0.8343(9) 0.26589(17) 0.075(2) Uani 1 1 d . . . H22A H 0.8416 -0.8626 0.2483 0.090 Uiso 1 1 calc R . . H22B H 0.7447 -0.8236 0.2549 0.090 Uiso 1 1 calc R . . B1 B 0.5000 0.3355(15) 0.2500 0.069(3) Uani 1 2 d S . . B2 B 0.8957(8) -0.3898(16) 0.5048(3) 0.035(3) Uani 0.50 1 d P . . F1 F 0.5629(4) 0.2373(7) 0.24057(18) 0.122(2) Uani 1 1 d . . . F2 F 0.5345(6) 0.4254(9) 0.2772(2) 0.173(3) Uani 1 1 d . . . F3 F 0.9028(7) -0.4381(17) 0.4737(3) 0.112(4) Uani 0.50 1 d P . . F4 F 0.8451(10) -0.285(2) 0.4989(4) 0.156(6) Uani 0.50 1 d P . . F5 F 0.9747(8) -0.3385(14) 0.5191(3) 0.121(4) Uani 0.50 1 d P . . F6 F 0.8788(11) -0.496(2) 0.5205(4) 0.159(6) 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 0.0546(3) 0.0472(3) 0.0385(3) -0.00094(18) -0.00209(19) 0.0017(2) O1 0.059(2) 0.048(2) 0.042(2) -0.0036(18) -0.0149(18) 0.0014(19) O2 0.090(3) 0.049(2) 0.037(2) 0.0012(18) 0.010(2) -0.009(2) N1 0.042(2) 0.039(3) 0.041(2) 0.0043(19) 0.003(2) 0.002(2) N2 0.043(2) 0.039(2) 0.042(2) 0.0035(19) 0.0104(19) 0.0031(19) N3 0.038(2) 0.038(2) 0.043(2) -0.0029(19) 0.0010(19) 0.0043(19) N4 0.060(3) 0.045(3) 0.046(3) 0.001(2) 0.018(2) -0.003(2) C1 0.067(4) 0.046(3) 0.035(3) -0.003(2) 0.002(3) 0.011(3) C2 0.058(4) 0.051(4) 0.055(4) 0.011(3) 0.020(3) 0.013(3) C3 0.043(3) 0.041(3) 0.050(3) 0.000(2) 0.013(2) 0.006(2) C4 0.054(3) 0.043(3) 0.040(3) -0.005(2) 0.004(3) 0.001(3) C5 0.055(3) 0.038(3) 0.045(3) -0.007(2) 0.002(3) 0.001(3) C6 0.033(3) 0.040(3) 0.041(3) -0.001(2) 0.003(2) 0.000(2) C7 0.058(3) 0.046(3) 0.038(3) -0.006(2) 0.004(3) 0.001(3) C8 0.064(4) 0.037(3) 0.051(3) -0.008(3) 0.009(3) 0.002(3) C9 0.034(3) 0.045(3) 0.038(3) -0.003(2) 0.002(2) 0.002(2) C10 0.054(3) 0.049(3) 0.046(3) 0.008(3) -0.004(3) 0.009(3) C11 0.058(4) 0.058(4) 0.039(3) 0.001(3) -0.005(3) 0.006(3) C12 0.051(3) 0.049(3) 0.041(3) -0.010(3) -0.010(3) 0.007(3) C13 0.042(3) 0.058(4) 0.065(4) -0.012(3) 0.000(3) 0.004(3) C14 0.038(3) 0.048(3) 0.051(3) -0.003(3) 0.007(2) 0.009(2) C15 0.046(3) 0.055(4) 0.042(3) 0.004(3) 0.004(2) 0.006(3) C16 0.050(3) 0.042(3) 0.045(3) 0.005(2) 0.009(3) 0.005(3) C17 0.047(3) 0.040(3) 0.041(3) 0.001(2) 0.014(2) 0.001(2) C18 0.071(4) 0.050(4) 0.042(3) 0.005(3) -0.002(3) 0.012(3) C19 0.079(4) 0.045(4) 0.055(4) 0.000(3) 0.002(3) 0.014(3) C20 0.048(3) 0.051(3) 0.037(3) 0.002(2) 0.011(2) 0.001(3) C21 0.083(5) 0.052(4) 0.049(4) -0.007(3) 0.021(3) -0.006(3) C22 0.115(6) 0.061(4) 0.048(4) -0.008(3) 0.013(4) -0.017(4) B1 0.105(10) 0.053(6) 0.051(6) 0.000 0.014(6) 0.000 B2 0.031(6) 0.040(6) 0.030(6) 0.015(5) -0.004(5) 0.002(5) F1 0.128(5) 0.095(4) 0.160(5) -0.007(4) 0.074(4) 0.005(3) F2 0.209(8) 0.160(7) 0.126(5) -0.078(5) -0.034(5) -0.021(6) F3 0.083(7) 0.188(13) 0.063(6) 0.005(7) 0.004(5) 0.007(7) F4 0.145(11) 0.186(15) 0.127(11) -0.084(11) -0.005(9) 0.022(11) F5 0.119(9) 0.090(7) 0.138(10) -0.016(7) -0.017(7) -0.022(7) F6 0.158(13) 0.199(15) 0.120(10) 0.025(10) 0.025(9) -0.089(12) _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 2.319(5) 1_545 ? Ag1 N4 2.362(5) 1_565 ? Ag1 N3 2.387(4) . ? Ag1 N2 2.431(4) . ? O1 C9 1.350(6) . ? O1 C11 1.446(7) . ? O2 C20 1.346(6) . ? O2 C22 1.449(8) . ? N1 C9 1.275(7) . ? N1 C10 1.481(7) . ? N1 Ag1 2.319(5) 1_565 ? N2 C2 1.467(7) . ? N2 C1 1.473(7) . ? N2 H2C 0.9100 . ? N3 C13 1.463(7) . ? N3 C12 1.468(7) . ? N3 H3A 0.9100 . ? N4 C20 1.270(7) . ? N4 C21 1.473(8) . ? N4 Ag1 2.362(5) 1_545 ? C1 C12 1.498(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.511(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.377(8) . ? C3 C4 1.392(8) . ? C4 C5 1.361(8) . ? C4 H4A 0.9300 . ? C5 C6 1.382(7) . ? C5 H5A 0.9300 . ? C6 C7 1.396(8) . ? C6 C9 1.462(7) . ? C7 C8 1.371(8) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C10 C11 1.516(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.507(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.375(8) . ? C14 C19 1.392(8) . ? C15 C16 1.368(8) . ? C15 H15A 0.9300 . ? C16 C17 1.378(8) . ? C16 H16A 0.9300 . ? C17 C18 1.387(8) . ? C17 C20 1.464(8) . ? C18 C19 1.355(9) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C22 1.517(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? B1 F2 1.322(9) 2_655 ? B1 F2 1.322(9) . ? B1 F1 1.355(9) . ? B1 F1 1.355(9) 2_655 ? B2 F6 1.125(17) . ? B2 F4 1.149(18) . ? B2 F3 1.299(16) . ? B2 F5 1.304(15) . ? 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 N4 91.70(17) 1_545 1_565 ? N1 Ag1 N3 126.61(16) 1_545 . ? N4 Ag1 N3 121.16(17) 1_565 . ? N1 Ag1 N2 119.58(15) 1_545 . ? N4 Ag1 N2 125.13(16) 1_565 . ? N3 Ag1 N2 76.79(14) . . ? C9 O1 C11 105.5(4) . . ? C20 O2 C22 105.8(5) . . ? C9 N1 C10 106.1(5) . . ? C9 N1 Ag1 126.7(4) . 1_565 ? C10 N1 Ag1 121.4(4) . 1_565 ? C2 N2 C1 111.8(4) . . ? C2 N2 Ag1 117.7(4) . . ? C1 N2 Ag1 103.7(3) . . ? C2 N2 H2C 107.7 . . ? C1 N2 H2C 107.7 . . ? Ag1 N2 H2C 107.7 . . ? C13 N3 C12 111.5(4) . . ? C13 N3 Ag1 117.6(4) . . ? C12 N3 Ag1 104.5(3) . . ? C13 N3 H3A 107.6 . . ? C12 N3 H3A 107.6 . . ? Ag1 N3 H3A 107.6 . . ? C20 N4 C21 106.4(5) . . ? C20 N4 Ag1 127.3(4) . 1_545 ? C21 N4 Ag1 122.3(4) . 1_545 ? N2 C1 C12 111.2(5) . . ? N2 C1 H1A 109.4 . . ? C12 C1 H1A 109.4 . . ? N2 C1 H1B 109.4 . . ? C12 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C3 110.8(5) . . ? N2 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C8 C3 C4 117.9(5) . . ? C8 C3 C2 121.5(5) . . ? C4 C3 C2 120.6(5) . . ? C5 C4 C3 120.9(5) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 121.1(5) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C5 C6 C7 118.6(5) . . ? C5 C6 C9 120.7(5) . . ? C7 C6 C9 120.6(5) . . ? C8 C7 C6 119.6(5) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C7 C8 C3 121.9(5) . . ? C7 C8 H8A 119.0 . . ? C3 C8 H8A 119.0 . . ? N1 C9 O1 118.1(5) . . ? N1 C9 C6 126.3(5) . . ? O1 C9 C6 115.6(5) . . ? N1 C10 C11 103.7(5) . . ? N1 C10 H10A 111.0 . . ? C11 C10 H10A 111.0 . . ? N1 C10 H10B 111.0 . . ? C11 C10 H10B 111.0 . . ? H10A C10 H10B 109.0 . . ? O1 C11 C10 104.1(4) . . ? O1 C11 H11A 110.9 . . ? C10 C11 H11A 110.9 . . ? O1 C11 H11B 110.9 . . ? C10 C11 H11B 110.9 . . ? H11A C11 H11B 109.0 . . ? N3 C12 C1 111.5(5) . . ? N3 C12 H12A 109.3 . . ? C1 C12 H12A 109.3 . . ? N3 C12 H12B 109.3 . . ? C1 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? N3 C13 C14 111.7(5) . . ? N3 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? N3 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C19 117.3(6) . . ? C15 C14 C13 121.7(5) . . ? C19 C14 C13 121.0(6) . . ? C16 C15 C14 121.7(5) . . ? C16 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C15 C16 C17 120.5(5) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C16 C17 C18 118.3(5) . . ? C16 C17 C20 120.2(5) . . ? C18 C17 C20 121.5(5) . . ? C19 C18 C17 120.8(6) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C14 121.4(6) . . ? C18 C19 H19A 119.3 . . ? C14 C19 H19A 119.3 . . ? N4 C20 O2 118.2(5) . . ? N4 C20 C17 126.4(5) . . ? O2 C20 C17 115.4(5) . . ? N4 C21 C22 104.1(5) . . ? N4 C21 H21A 110.9 . . ? C22 C21 H21A 110.9 . . ? N4 C21 H21B 110.9 . . ? C22 C21 H21B 110.9 . . ? H21A C21 H21B 108.9 . . ? O2 C22 C21 103.9(5) . . ? O2 C22 H22A 111.0 . . ? C21 C22 H22A 111.0 . . ? O2 C22 H22B 111.0 . . ? C21 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? F2 B1 F2 112.0(12) 2_655 . ? F2 B1 F1 108.3(5) 2_655 . ? F2 B1 F1 110.7(5) . . ? F2 B1 F1 110.7(5) 2_655 2_655 ? F2 B1 F1 108.3(5) . 2_655 ? F1 B1 F1 106.8(10) . 2_655 ? F6 B2 F4 118.6(17) . . ? F6 B2 F3 109.8(15) . . ? F4 B2 F3 102.0(11) . . ? F6 B2 F5 107.6(13) . . ? F4 B2 F5 112.3(14) . . ? F3 B2 F5 105.7(12) . . ? 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 N2 C2 -14.0(4) 1_545 . . . ? N4 Ag1 N2 C2 102.2(4) 1_565 . . . ? N3 Ag1 N2 C2 -138.8(4) . . . . ? N1 Ag1 N2 C1 110.1(4) 1_545 . . . ? N4 Ag1 N2 C1 -133.8(3) 1_565 . . . ? N3 Ag1 N2 C1 -14.8(3) . . . . ? N1 Ag1 N3 C13 102.1(4) 1_545 . . . ? N4 Ag1 N3 C13 -17.4(5) 1_565 . . . ? N2 Ag1 N3 C13 -140.7(4) . . . . ? N1 Ag1 N3 C12 -133.7(3) 1_545 . . . ? N4 Ag1 N3 C12 106.8(4) 1_565 . . . ? N2 Ag1 N3 C12 -16.5(3) . . . . ? C2 N2 C1 C12 173.2(5) . . . . ? Ag1 N2 C1 C12 45.4(5) . . . . ? C1 N2 C2 C3 167.9(5) . . . . ? Ag1 N2 C2 C3 -72.2(6) . . . . ? N2 C2 C3 C8 65.1(7) . . . . ? N2 C2 C3 C4 -114.2(6) . . . . ? C8 C3 C4 C5 -1.1(9) . . . . ? C2 C3 C4 C5 178.2(5) . . . . ? C3 C4 C5 C6 0.8(9) . . . . ? C4 C5 C6 C7 0.7(8) . . . . ? C4 C5 C6 C9 -178.4(5) . . . . ? C5 C6 C7 C8 -1.9(9) . . . . ? C9 C6 C7 C8 177.1(5) . . . . ? C6 C7 C8 C3 1.7(9) . . . . ? C4 C3 C8 C7 -0.2(9) . . . . ? C2 C3 C8 C7 -179.4(6) . . . . ? C10 N1 C9 O1 4.5(7) . . . . ? Ag1 N1 C9 O1 -148.6(4) 1_565 . . . ? C10 N1 C9 C6 -173.9(5) . . . . ? Ag1 N1 C9 C6 33.0(8) 1_565 . . . ? C11 O1 C9 N1 6.1(7) . . . . ? C11 O1 C9 C6 -175.3(5) . . . . ? C5 C6 C9 N1 25.9(8) . . . . ? C7 C6 C9 N1 -153.2(6) . . . . ? C5 C6 C9 O1 -152.6(5) . . . . ? C7 C6 C9 O1 28.4(7) . . . . ? C9 N1 C10 C11 -12.5(6) . . . . ? Ag1 N1 C10 C11 142.3(4) 1_565 . . . ? C9 O1 C11 C10 -13.4(6) . . . . ? N1 C10 C11 O1 15.7(6) . . . . ? C13 N3 C12 C1 175.6(5) . . . . ? Ag1 N3 C12 C1 47.6(5) . . . . ? N2 C1 C12 N3 -68.1(7) . . . . ? C12 N3 C13 C14 169.0(5) . . . . ? Ag1 N3 C13 C14 -70.4(6) . . . . ? N3 C13 C14 C15 -111.3(6) . . . . ? N3 C13 C14 C19 69.2(8) . . . . ? C19 C14 C15 C16 -0.5(9) . . . . ? C13 C14 C15 C16 180.0(5) . . . . ? C14 C15 C16 C17 -1.1(9) . . . . ? C15 C16 C17 C18 1.8(8) . . . . ? C15 C16 C17 C20 -179.7(5) . . . . ? C16 C17 C18 C19 -1.0(10) . . . . ? C20 C17 C18 C19 -179.4(6) . . . . ? C17 C18 C19 C14 -0.7(11) . . . . ? C15 C14 C19 C18 1.4(10) . . . . ? C13 C14 C19 C18 -179.1(6) . . . . ? C21 N4 C20 O2 4.9(7) . . . . ? Ag1 N4 C20 O2 -152.8(4) 1_545 . . . ? C21 N4 C20 C17 -174.7(6) . . . . ? Ag1 N4 C20 C17 27.6(9) 1_545 . . . ? C22 O2 C20 N4 3.3(8) . . . . ? C22 O2 C20 C17 -177.2(6) . . . . ? C16 C17 C20 N4 26.5(9) . . . . ? C18 C17 C20 N4 -155.0(6) . . . . ? C16 C17 C20 O2 -153.0(5) . . . . ? C18 C17 C20 O2 25.4(8) . . . . ? C20 N4 C21 C22 -10.4(7) . . . . ? Ag1 N4 C21 C22 148.7(5) 1_545 . . . ? C20 O2 C22 C21 -9.4(7) . . . . ? N4 C21 C22 O2 11.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.290 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.114 #====END data_6 _database_code_depnum_ccdc_archive 'CCDC 765661' #TrackingRef '- NJ-ART-02-2010-000092R1.cif' _audit_creation_date 'Wed Dec 28 20:00:19 2005' _audit_creation_method SHELXL-97 _publ_section_references ; Molecular Structure Corporation, Rigaku Corporation. (2004). teXsan. Single Crystal Structure Analysis Software. Version 2.0. MSC, 9009 New Trails Drive, The Woodlands, TX 77381-5209, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _chemical_name_systematic ; [Cu4(L)2(OCH3)2(OH)2](NO3)2-0.32(H2O) ; _chemical_name_common (Cu4(L)2(OCH3)2(OH)2)(NO3)2-0.32(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C46 H60.64 Cu4 N12 O20.32 ' _chemical_formula_sum 'C46 H60.64 Cu4 N12 O20.63' _chemical_formula_weight 1360.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.3839(19) _cell_length_b 15.715(2) _cell_length_c 26.095(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.420(5) _cell_angle_gamma 90.00 _cell_volume 5472.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 32711 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _exptl_crystal_description platelet _exptl_crystal_colour blue _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.100 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2823 _exptl_absorpt_coefficient_mu 1.622 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.495 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 39744 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9628 _reflns_number_gt 7327 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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. The nitrate anions (N04, O41, O42, O43; N04B, O41B, O42B, O43B) near the special position (1/2, 1/2, 1/2) are highly disordered. In the refinement process, the geometry was deformed and the thermal factors became unreasonable or negative values. Thus the geometry of the anions was restrained by the SADI instruction in SHELXL-97 for N-O and O-O distances. The thermal factors of the oxygen atoms in the anions were restrained using ISOR and DELU instructions. ; _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^)+(0.0527P)^2^+39.0896P] 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 9628 _refine_ls_number_parameters 775 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.1904 _refine_ls_wR_factor_gt 0.1795 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.102 _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 Cu1 Cu 0.20563(6) 0.47846(5) 0.87756(3) 0.0297(2) Uani 1 1 d . . . Cu2 Cu 0.35820(6) 0.61235(5) 0.87178(3) 0.0307(2) Uani 1 1 d . . . Cu3 Cu 0.13385(6) 0.48675(5) 0.60727(3) 0.0319(2) Uani 1 1 d . . . Cu4 Cu 0.29040(6) 0.60834(5) 0.60293(3) 0.0321(2) Uani 1 1 d . . . O13 O 0.3149(5) 0.5587(4) 1.0343(2) 0.0628(18) Uani 1 1 d . . . O12 O 0.3532(5) 0.6035(4) 0.9611(2) 0.0545(16) Uani 1 1 d . . . O11 O 0.2437(4) 0.5019(4) 0.96689(19) 0.0476(14) Uani 1 1 d . . . O31 O 0.0304(6) 0.7266(7) 0.5533(4) 0.110(3) Uani 1 1 d . . . O32 O 0.1321(6) 0.7693(6) 0.5015(3) 0.094(3) Uani 1 1 d . . . O33 O -0.0241(6) 0.7894(7) 0.4832(3) 0.101(3) Uani 1 1 d . . . O21 O 0.1349(4) 0.4882(4) 0.5156(2) 0.0539(15) Uani 1 1 d . . . O22 O 0.2654(5) 0.5736(4) 0.5145(2) 0.0610(18) Uani 1 1 d . . . O23 O 0.2401(5) 0.4751(4) 0.4571(2) 0.0589(16) Uani 1 1 d . . . O41 O 0.4013(9) 0.3680(13) 0.5741(5) 0.117(7) Uani 0.631(12) 1 d PDU . . O41B O 0.3553(18) 0.3769(13) 0.5596(8) 0.085(7) Uani 0.369(12) 1 d PDU . . O42 O 0.4249(5) 0.3119(6) 0.5010(3) 0.088(2) Uani 1 1 d DU . . O43 O 0.2807(7) 0.3092(8) 0.5310(3) 0.077(4) Uani 0.631(12) 1 d PDU . . O43B O 0.443(2) 0.4459(9) 0.5092(9) 0.108(9) Uani 0.369(12) 1 d PDU . . O51 O 0.2144(3) 0.5974(3) 0.85816(17) 0.0324(10) Uani 1 1 d . . . O52 O 0.3457(4) 0.4895(3) 0.86368(18) 0.0336(11) Uani 1 1 d . . . O61 O 0.1497(4) 0.6089(3) 0.61564(18) 0.0354(11) Uani 1 1 d . . . O62 O 0.2777(4) 0.4900(3) 0.62321(19) 0.0360(11) Uani 1 1 d . . . O71 O 0.5000 0.5000 0.5000 0.146(11) Uani 0.631(12) 2 d SP . . O101 O -0.1093(4) 0.4791(4) 0.8733(2) 0.0546(16) Uani 1 1 d . . . O201 O 0.1982(4) 0.2135(3) 0.8722(2) 0.0469(13) Uani 1 1 d . . . O301 O 0.6687(4) 0.6183(4) 0.8619(2) 0.0561(16) Uani 1 1 d . . . O401 O 0.3571(4) 0.8781(3) 0.85580(18) 0.0410(12) Uani 1 1 d . . . N1 N -0.0181(5) 0.4913(4) 0.5967(2) 0.0378(14) Uani 1 1 d . . . H1 H -0.0308 0.5190 0.5654 0.045 Uiso 1 1 calc R . . N01 N 0.3039(5) 0.5556(4) 0.9872(2) 0.0365(14) Uani 1 1 d . . . N2 N 0.1144(5) 0.3585(4) 0.6040(2) 0.0400(14) Uani 1 1 d . . . H2 H 0.1178 0.3442 0.5696 0.048 Uiso 1 1 calc R . . N03 N 0.0459(6) 0.7620(6) 0.5119(3) 0.059(2) Uani 1 1 d . . . N3 N 0.4408(4) 0.6129(4) 0.5971(2) 0.0360(14) Uani 1 1 d . . . H3 H 0.4483 0.6017 0.5626 0.043 Uiso 1 1 calc R . . N02 N 0.2145(5) 0.5107(4) 0.4966(2) 0.0449(16) Uani 1 1 d . . . N4 N 0.2938(5) 0.7337(4) 0.5850(2) 0.0351(13) Uani 1 1 d . . . H4 H 0.2541 0.7387 0.5543 0.042 Uiso 1 1 calc R . . N04 N 0.3683(6) 0.3334(8) 0.5344(4) 0.054(3) Uani 0.631(12) 1 d PD . . N04B N 0.4068(14) 0.3785(7) 0.5227(6) 0.068(7) Uani 0.369(12) 1 d PD . . N101 N 0.0576(5) 0.4811(4) 0.8833(2) 0.0370(14) Uani 1 1 d . . . N201 N 0.2115(5) 0.3532(4) 0.8874(2) 0.0354(13) Uani 1 1 d . . . N301 N 0.5084(5) 0.6130(4) 0.8773(2) 0.0403(15) Uani 1 1 d . . . N401 N 0.3522(4) 0.7396(4) 0.8726(2) 0.0320(13) Uani 1 1 d . . . C1 C -0.0582(7) 0.4045(5) 0.5874(4) 0.058(2) Uani 1 1 d . . . H5 H -0.1268 0.4008 0.5990 0.070 Uiso 1 1 calc R . . H6 H -0.0618 0.3918 0.5502 0.070 Uiso 1 1 calc R . . C2 C 0.0064(6) 0.3429(6) 0.6152(4) 0.057(2) Uani 1 1 d . . . H7 H -0.0138 0.2845 0.6046 0.068 Uiso 1 1 calc R . . H8 H -0.0004 0.3483 0.6526 0.068 Uiso 1 1 calc R . . C3 C 0.4715(6) 0.7033(5) 0.6039(3) 0.0381(17) Uani 1 1 d . . . H9 H 0.5394 0.7122 0.5922 0.046 Uiso 1 1 calc R . . H10 H 0.4722 0.7200 0.6405 0.046 Uiso 1 1 calc R . . C4 C 0.3956(6) 0.7553(5) 0.5719(3) 0.0410(18) Uani 1 1 d . . . H11 H 0.4083 0.8166 0.5782 0.049 Uiso 1 1 calc R . . H12 H 0.4021 0.7439 0.5350 0.049 Uiso 1 1 calc R . . C10 C -0.0714(6) 0.5434(5) 0.6336(3) 0.0389(17) Uani 1 1 d . . . H13 H -0.1442 0.5405 0.6238 0.047 Uiso 1 1 calc R . . H14 H -0.0504 0.6035 0.6305 0.047 Uiso 1 1 calc R . . C11 C -0.0532(5) 0.5167(5) 0.6895(3) 0.0372(16) Uani 1 1 d . . . C12 C -0.1293(6) 0.4819(6) 0.7157(3) 0.051(2) Uani 1 1 d . . . H15 H -0.1910 0.4677 0.6973 0.061 Uiso 1 1 calc R . . C13 C -0.1174(6) 0.4671(6) 0.7683(3) 0.052(2) Uani 1 1 d . . . H16 H -0.1704 0.4424 0.7854 0.063 Uiso 1 1 calc R . . C14 C -0.0283(5) 0.4885(5) 0.7958(3) 0.0374(17) Uani 1 1 d . . . C15 C 0.0499(5) 0.5213(5) 0.7695(3) 0.0385(17) Uani 1 1 d . . . H17 H 0.1124 0.5334 0.7877 0.046 Uiso 1 1 calc R . . C16 C 0.0375(5) 0.5362(5) 0.7176(3) 0.0371(16) Uani 1 1 d . . . H18 H 0.0909 0.5601 0.7005 0.044 Uiso 1 1 calc R . . C20 C 0.1823(6) 0.2970(5) 0.6333(3) 0.0377(16) Uani 1 1 d . . . H19 H 0.2519 0.3077 0.6247 0.045 Uiso 1 1 calc R . . H20 H 0.1641 0.2386 0.6218 0.045 Uiso 1 1 calc R . . C21 C 0.1789(5) 0.3014(5) 0.6907(3) 0.0373(16) Uani 1 1 d . . . C22 C 0.1255(6) 0.2409(5) 0.7168(3) 0.0454(19) Uani 1 1 d . . . H21 H 0.0853 0.2001 0.6979 0.054 Uiso 1 1 calc R . . C23 C 0.1306(6) 0.2399(5) 0.7696(3) 0.0462(19) Uani 1 1 d . . . H22 H 0.0953 0.1972 0.7867 0.055 Uiso 1 1 calc R . . C24 C 0.1860(6) 0.2994(5) 0.7983(3) 0.0383(17) Uani 1 1 d . . . C25 C 0.2376(6) 0.3625(5) 0.7723(3) 0.0438(19) Uani 1 1 d . . . H23 H 0.2757 0.4047 0.7912 0.053 Uiso 1 1 calc R . . C26 C 0.2324(6) 0.3625(5) 0.7195(3) 0.0418(18) Uani 1 1 d . . . H24 H 0.2666 0.4056 0.7023 0.050 Uiso 1 1 calc R . . C30 C 0.5123(5) 0.5535(5) 0.6253(3) 0.0378(17) Uani 1 1 d . . . H25 H 0.5781 0.5576 0.6106 0.045 Uiso 1 1 calc R . . H26 H 0.4876 0.4945 0.6201 0.045 Uiso 1 1 calc R . . C31 C 0.5260(5) 0.5716(4) 0.6822(3) 0.0373(16) Uani 1 1 d . . . C32 C 0.6141(6) 0.6071(6) 0.7040(3) 0.049(2) Uani 1 1 d . . . H27 H 0.6652 0.6225 0.6823 0.058 Uiso 1 1 calc R . . C33 C 0.6295(6) 0.6208(6) 0.7560(3) 0.049(2) Uani 1 1 d . . . H28 H 0.6909 0.6447 0.7699 0.059 Uiso 1 1 calc R . . C34 C 0.5552(5) 0.5996(5) 0.7885(3) 0.0397(17) Uani 1 1 d . . . C35 C 0.4661(6) 0.5628(5) 0.7667(3) 0.0415(18) Uani 1 1 d . . . H29 H 0.4148 0.5471 0.7881 0.050 Uiso 1 1 calc R . . C36 C 0.4526(6) 0.5493(5) 0.7143(3) 0.0421(18) Uani 1 1 d . . . H30 H 0.3920 0.5244 0.7001 0.050 Uiso 1 1 calc R . . C40 C 0.2502(6) 0.7955(4) 0.6207(2) 0.0355(16) Uani 1 1 d . . . H31 H 0.1766 0.7876 0.6184 0.043 Uiso 1 1 calc R . . H32 H 0.2636 0.8538 0.6087 0.043 Uiso 1 1 calc R . . C41 C 0.2890(6) 0.7885(4) 0.6766(3) 0.0338(16) Uani 1 1 d . . . C42 C 0.3487(6) 0.8521(5) 0.6991(3) 0.0380(17) Uani 1 1 d . . . H33 H 0.3735 0.8955 0.6782 0.046 Uiso 1 1 calc R . . C43 C 0.3729(6) 0.8537(5) 0.7514(3) 0.0374(16) Uani 1 1 d . . . H34 H 0.4134 0.8983 0.7663 0.045 Uiso 1 1 calc R . . C44 C 0.3378(6) 0.7895(4) 0.7825(3) 0.0343(16) Uani 1 1 d . . . C45 C 0.2818(6) 0.7236(5) 0.7598(3) 0.0404(18) Uani 1 1 d . . . H35 H 0.2603 0.6782 0.7803 0.049 Uiso 1 1 calc R . . C46 C 0.2573(6) 0.7237(5) 0.7076(3) 0.0388(17) Uani 1 1 d . . . H36 H 0.2180 0.6785 0.6925 0.047 Uiso 1 1 calc R . . C51 C 0.1457(6) 0.6595(5) 0.8720(3) 0.0464(19) Uani 1 1 d . . . H37 H 0.0772 0.6388 0.8639 0.056 Uiso 1 1 calc R . . H38 H 0.1559 0.7121 0.8529 0.056 Uiso 1 1 calc R . . H39 H 0.1560 0.6708 0.9090 0.056 Uiso 1 1 calc R . . C52 C 0.4214(6) 0.4322(5) 0.8836(4) 0.055(2) Uani 1 1 d . . . H40 H 0.4219 0.4304 0.9211 0.066 Uiso 1 1 calc R . . H41 H 0.4868 0.4516 0.8738 0.066 Uiso 1 1 calc R . . H42 H 0.4076 0.3752 0.8695 0.066 Uiso 1 1 calc R . . C101 C -0.0222(6) 0.4815(5) 0.8523(3) 0.0416(18) Uani 1 1 d . . . C102 C -0.0878(7) 0.4804(9) 0.9290(4) 0.073(3) Uani 1 1 d . . . H43 H -0.1154 0.4292 0.9450 0.087 Uiso 1 1 calc R . . H44 H -0.1167 0.5317 0.9441 0.087 Uiso 1 1 calc R . . C103 C 0.0230(6) 0.4815(7) 0.9365(3) 0.052(2) Uani 1 1 d . . . H45 H 0.0481 0.4308 0.9559 0.062 Uiso 1 1 calc R . . H46 H 0.0467 0.5333 0.9554 0.062 Uiso 1 1 calc R . . C201 C 0.1988(6) 0.2932(5) 0.8543(3) 0.0394(17) Uani 1 1 d . . . C202 C 0.2110(7) 0.2191(5) 0.9285(3) 0.0461(19) Uani 1 1 d . . . H47 H 0.2695 0.1852 0.9422 0.055 Uiso 1 1 calc R . . H48 H 0.1504 0.1984 0.9441 0.055 Uiso 1 1 calc R . . C203 C 0.2274(7) 0.3122(5) 0.9392(3) 0.049(2) Uani 1 1 d . . . H49 H 0.1788 0.3340 0.9628 0.059 Uiso 1 1 calc R . . H50 H 0.2962 0.3228 0.9546 0.059 Uiso 1 1 calc R . . C301 C 0.5731(6) 0.6108(5) 0.8442(3) 0.0418(18) Uani 1 1 d . . . C302 C 0.6713(7) 0.6267(7) 0.9173(3) 0.065(3) Uani 1 1 d . . . H51 H 0.7001 0.6823 0.9286 0.078 Uiso 1 1 calc R . . H52 H 0.7114 0.5806 0.9346 0.078 Uiso 1 1 calc R . . C303 C 0.5635(6) 0.6205(6) 0.9288(3) 0.054(2) Uani 1 1 d . . . H53 H 0.5522 0.5698 0.9502 0.065 Uiso 1 1 calc R . . H54 H 0.5424 0.6719 0.9471 0.065 Uiso 1 1 calc R . . C401 C 0.3512(5) 0.7975(4) 0.8387(3) 0.0316(15) Uani 1 1 d . . . C402 C 0.3682(6) 0.8742(5) 0.9117(3) 0.0429(18) Uani 1 1 d . . . H55 H 0.3175 0.9102 0.9269 0.051 Uiso 1 1 calc R . . H56 H 0.4358 0.8933 0.9249 0.051 Uiso 1 1 calc R . . C403 C 0.3527(6) 0.7822(5) 0.9238(3) 0.0407(18) Uani 1 1 d . . . H57 H 0.4079 0.7603 0.9476 0.049 Uiso 1 1 calc R . . H58 H 0.2883 0.7735 0.9393 0.049 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 Cu1 0.0310(4) 0.0285(4) 0.0298(4) 0.0014(3) 0.0027(3) -0.0036(4) Cu2 0.0335(5) 0.0283(4) 0.0298(4) 0.0017(3) -0.0008(3) -0.0043(4) Cu3 0.0349(5) 0.0302(5) 0.0308(4) -0.0034(3) 0.0038(4) -0.0037(4) Cu4 0.0361(5) 0.0309(5) 0.0295(4) -0.0031(3) 0.0039(3) -0.0048(4) O13 0.087(5) 0.064(4) 0.038(3) -0.009(3) 0.013(3) -0.030(4) O12 0.073(4) 0.056(4) 0.034(3) 0.005(3) 0.002(3) -0.032(3) O11 0.058(4) 0.048(3) 0.036(3) -0.006(2) 0.003(3) -0.020(3) O31 0.058(5) 0.163(9) 0.109(7) 0.065(7) 0.001(5) 0.007(5) O32 0.066(5) 0.157(9) 0.058(4) 0.017(5) -0.005(4) -0.008(5) O33 0.078(5) 0.159(9) 0.064(5) 0.014(5) -0.005(4) 0.037(6) O21 0.051(3) 0.073(4) 0.039(3) 0.007(3) 0.011(3) -0.013(3) O22 0.093(5) 0.060(4) 0.031(3) -0.014(3) 0.012(3) -0.037(4) O23 0.082(4) 0.053(4) 0.043(3) -0.016(3) 0.012(3) -0.011(3) O41 0.056(8) 0.157(13) 0.144(13) -0.079(11) 0.037(7) -0.002(8) O41B 0.059(11) 0.095(14) 0.107(14) -0.021(10) 0.052(9) 0.010(9) O42 0.068(5) 0.115(7) 0.080(5) -0.029(5) -0.002(4) 0.034(5) O43 0.074(7) 0.114(9) 0.043(6) 0.003(5) 0.009(5) 0.007(6) O43B 0.103(16) 0.119(17) 0.100(15) 0.020(14) -0.003(12) -0.028(13) O51 0.035(3) 0.028(2) 0.034(2) 0.000(2) 0.001(2) 0.001(2) O52 0.034(3) 0.028(2) 0.039(3) 0.003(2) 0.004(2) 0.002(2) O61 0.037(3) 0.031(3) 0.038(3) -0.006(2) 0.006(2) -0.004(2) O62 0.034(3) 0.030(3) 0.044(3) -0.001(2) 0.001(2) -0.005(2) O71 0.17(3) 0.14(3) 0.13(2) 0.008(19) -0.01(2) 0.01(2) O101 0.035(3) 0.090(5) 0.039(3) 0.010(3) 0.005(2) -0.003(3) O201 0.070(4) 0.030(3) 0.041(3) 0.005(2) 0.005(3) -0.007(3) O301 0.032(3) 0.081(4) 0.053(3) 0.006(3) -0.007(3) -0.010(3) O401 0.065(4) 0.030(3) 0.028(2) -0.003(2) 0.005(2) -0.004(2) N1 0.041(4) 0.032(3) 0.040(3) -0.007(3) 0.004(3) -0.003(3) N01 0.040(3) 0.036(3) 0.032(3) -0.003(3) 0.000(3) -0.002(3) N2 0.044(4) 0.033(3) 0.042(3) -0.005(3) -0.002(3) 0.002(3) N03 0.047(5) 0.082(6) 0.048(4) -0.003(4) 0.000(4) 0.008(4) N3 0.040(3) 0.034(3) 0.035(3) -0.005(3) 0.010(3) -0.001(3) N02 0.062(4) 0.042(4) 0.030(3) -0.002(3) 0.002(3) -0.007(3) N4 0.042(3) 0.041(3) 0.023(3) 0.001(2) 0.002(2) -0.007(3) N04 0.049(8) 0.041(7) 0.071(9) -0.011(6) 0.000(7) 0.006(6) N04B 0.046(14) 0.062(16) 0.09(2) 0.017(15) -0.014(13) 0.007(13) N101 0.037(3) 0.043(4) 0.032(3) -0.001(3) 0.004(3) -0.005(3) N201 0.041(3) 0.030(3) 0.036(3) 0.002(3) 0.005(3) -0.001(3) N301 0.035(3) 0.044(4) 0.040(3) 0.008(3) -0.009(3) -0.009(3) N401 0.037(3) 0.034(3) 0.024(3) -0.001(2) -0.002(2) -0.010(3) C1 0.047(5) 0.040(5) 0.085(7) -0.016(4) -0.001(5) -0.005(4) C2 0.047(5) 0.052(5) 0.071(6) 0.004(4) -0.004(4) -0.015(4) C3 0.042(4) 0.034(4) 0.040(4) 0.004(3) 0.011(3) -0.006(3) C4 0.041(4) 0.043(4) 0.039(4) 0.009(3) 0.004(3) -0.009(4) C10 0.038(4) 0.042(4) 0.035(4) -0.005(3) -0.001(3) 0.008(3) C11 0.035(4) 0.041(4) 0.034(4) 0.000(3) -0.003(3) -0.001(3) C12 0.039(4) 0.065(6) 0.047(5) 0.006(4) -0.009(4) -0.016(4) C13 0.040(4) 0.069(6) 0.047(5) 0.012(4) 0.000(4) -0.018(4) C14 0.030(4) 0.049(4) 0.033(4) 0.005(3) -0.001(3) -0.002(3) C15 0.033(4) 0.048(4) 0.035(4) -0.005(3) 0.000(3) -0.006(3) C16 0.037(4) 0.039(4) 0.036(4) 0.002(3) 0.009(3) -0.003(3) C20 0.043(4) 0.032(4) 0.038(4) -0.003(3) 0.004(3) 0.001(3) C21 0.038(4) 0.033(4) 0.041(4) -0.003(3) 0.005(3) 0.002(3) C22 0.053(5) 0.036(4) 0.047(5) 0.001(3) -0.003(4) -0.015(4) C23 0.052(5) 0.039(4) 0.047(5) 0.006(4) 0.004(4) -0.019(4) C24 0.046(4) 0.031(4) 0.039(4) -0.002(3) 0.008(3) 0.001(3) C25 0.057(5) 0.033(4) 0.041(4) -0.005(3) 0.005(4) -0.013(4) C26 0.052(5) 0.033(4) 0.041(4) -0.002(3) 0.011(4) -0.009(4) C30 0.035(4) 0.035(4) 0.044(4) -0.001(3) 0.004(3) 0.002(3) C31 0.039(4) 0.027(4) 0.046(4) 0.004(3) 0.008(3) 0.005(3) C32 0.034(4) 0.056(5) 0.056(5) 0.008(4) 0.006(4) -0.006(4) C33 0.038(4) 0.058(5) 0.050(5) 0.003(4) 0.001(4) -0.015(4) C34 0.035(4) 0.035(4) 0.049(4) 0.006(3) 0.003(3) -0.005(3) C35 0.032(4) 0.048(5) 0.045(4) 0.007(4) 0.006(3) -0.006(3) C36 0.039(4) 0.041(4) 0.046(4) 0.001(3) 0.000(3) -0.008(3) C40 0.049(4) 0.031(4) 0.028(3) 0.003(3) 0.005(3) 0.007(3) C41 0.046(4) 0.029(4) 0.028(3) -0.002(3) 0.006(3) 0.007(3) C42 0.049(4) 0.030(4) 0.036(4) 0.006(3) 0.013(3) -0.008(3) C43 0.048(4) 0.032(4) 0.032(4) -0.002(3) 0.000(3) -0.009(3) C44 0.044(4) 0.030(4) 0.029(3) -0.002(3) 0.005(3) 0.004(3) C45 0.059(5) 0.027(4) 0.035(4) -0.001(3) 0.008(4) -0.006(4) C46 0.055(5) 0.034(4) 0.028(4) -0.002(3) 0.003(3) -0.010(4) C51 0.039(4) 0.043(4) 0.058(5) -0.005(4) 0.008(4) 0.001(4) C52 0.046(5) 0.037(4) 0.083(6) 0.009(4) 0.014(4) 0.012(4) C101 0.045(4) 0.044(4) 0.036(4) 0.006(3) 0.009(3) -0.009(4) C102 0.041(5) 0.130(10) 0.048(5) 0.002(6) 0.009(4) -0.010(6) C103 0.041(4) 0.079(6) 0.036(4) 0.004(4) 0.010(4) -0.008(4) C201 0.037(4) 0.036(4) 0.046(4) 0.001(3) 0.008(3) -0.003(3) C202 0.055(5) 0.041(4) 0.043(4) 0.008(3) 0.001(4) -0.006(4) C203 0.063(5) 0.041(4) 0.042(4) 0.008(4) 0.002(4) -0.010(4) C301 0.042(4) 0.034(4) 0.049(4) 0.008(3) 0.003(4) -0.007(3) C302 0.050(5) 0.093(8) 0.048(5) 0.023(5) -0.011(4) -0.026(5) C303 0.043(5) 0.073(6) 0.045(5) 0.000(4) -0.010(4) -0.013(4) C401 0.036(4) 0.030(4) 0.029(3) -0.003(3) 0.001(3) -0.002(3) C402 0.061(5) 0.041(4) 0.026(4) -0.005(3) 0.002(3) -0.009(4) C403 0.056(5) 0.038(4) 0.029(4) -0.005(3) 0.006(3) -0.008(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 Cu1 O51 1.943(5) . ? Cu1 O52 1.945(5) . ? Cu1 N201 1.985(6) . ? Cu1 N101 1.999(6) . ? Cu1 O11 2.376(5) . ? Cu1 Cu2 2.9439(12) . ? Cu2 O51 1.944(5) . ? Cu2 O52 1.948(5) . ? Cu2 N401 2.001(6) . ? Cu2 N301 2.004(6) . ? Cu2 O12 2.340(5) . ? Cu3 O62 1.939(5) . ? Cu3 O61 1.942(5) . ? Cu3 N1 2.033(6) . ? Cu3 N2 2.033(6) . ? Cu3 O21 2.393(5) . ? Cu3 Cu4 2.8444(12) . ? Cu4 O61 1.937(5) . ? Cu4 O62 1.945(5) . ? Cu4 N4 2.027(6) . ? Cu4 N3 2.032(6) . ? Cu4 O22 2.371(5) . ? O13 N01 1.228(8) . ? O12 N01 1.240(8) . ? O11 N01 1.255(8) . ? O31 N03 1.245(10) . ? O32 N03 1.211(10) . ? O33 N03 1.232(10) . ? O21 N02 1.260(8) . ? O22 N02 1.268(8) . ? O23 N02 1.243(8) . ? O41 N04 1.221(8) . ? O41B N04B 1.229(8) . ? O42 N04B 1.223(8) . ? O42 N04 1.245(8) . ? O43 N04 1.230(8) . ? O43B O71 1.181(17) . ? O43B N04B 1.226(8) . ? O51 C51 1.407(9) . ? O52 C52 1.422(9) . ? O71 O43B 1.181(17) 3_666 ? O101 C101 1.327(9) . ? O101 C102 1.459(10) . ? O201 C201 1.337(9) . ? O201 C202 1.470(9) . ? O301 C301 1.331(9) . ? O301 C302 1.451(10) . ? O401 C401 1.342(8) . ? O401 C402 1.456(8) . ? N1 C1 1.478(10) . ? N1 C10 1.488(9) . ? N1 H1 0.9300 . ? N2 C20 1.495(9) . ? N2 C2 1.518(10) . ? N2 H2 0.9300 . ? N3 C3 1.486(9) . ? N3 C30 1.489(9) . ? N3 H3 0.9300 . ? N4 C4 1.471(9) . ? N4 C40 1.494(9) . ? N4 H4 0.9300 . ? N101 C101 1.289(10) . ? N101 C103 1.498(9) . ? N201 C201 1.280(9) . ? N201 C203 1.499(9) . ? N301 C301 1.272(10) . ? N301 C303 1.487(10) . ? N401 C401 1.268(9) . ? N401 C403 1.494(9) . ? C1 C2 1.455(13) . ? C1 H5 0.9900 . ? C1 H6 0.9900 . ? C2 H7 0.9900 . ? C2 H8 0.9900 . ? C3 C4 1.505(10) . ? C3 H9 0.9900 . ? C3 H10 0.9900 . ? C4 H11 0.9900 . ? C4 H12 0.9900 . ? C10 C11 1.519(10) . ? C10 H13 0.9900 . ? C10 H14 0.9900 . ? C11 C12 1.381(11) . ? C11 C16 1.403(10) . ? C12 C13 1.390(11) . ? C12 H15 0.9500 . ? C13 C14 1.386(11) . ? C13 H16 0.9500 . ? C14 C15 1.393(10) . ? C14 C101 1.473(10) . ? C15 C16 1.371(10) . ? C15 H17 0.9500 . ? C16 H18 0.9500 . ? C20 C21 1.505(10) . ? C20 H19 0.9900 . ? C20 H20 0.9900 . ? C21 C26 1.385(10) . ? C21 C22 1.397(10) . ? C22 C23 1.374(11) . ? C22 H21 0.9500 . ? C23 C24 1.378(10) . ? C23 H22 0.9500 . ? C24 C25 1.413(10) . ? C24 C201 1.461(10) . ? C25 C26 1.374(11) . ? C25 H23 0.9500 . ? C26 H24 0.9500 . ? C30 C31 1.511(10) . ? C30 H25 0.9900 . ? C30 H26 0.9900 . ? C31 C36 1.383(10) . ? C31 C32 1.387(11) . ? C32 C33 1.374(12) . ? C32 H27 0.9500 . ? C33 C34 1.396(11) . ? C33 H28 0.9500 . ? C34 C35 1.405(10) . ? C34 C301 1.466(11) . ? C35 C36 1.382(11) . ? C35 H29 0.9500 . ? C36 H30 0.9500 . ? C40 C41 1.515(9) . ? C40 H31 0.9900 . ? C40 H32 0.9900 . ? C41 C42 1.382(10) . ? C41 C46 1.387(10) . ? C42 C43 1.379(10) . ? C42 H33 0.9500 . ? C43 C44 1.398(10) . ? C43 H34 0.9500 . ? C44 C45 1.383(10) . ? C44 C401 1.471(9) . ? C45 C46 1.376(10) . ? C45 H35 0.9500 . ? C46 H36 0.9500 . ? C51 H37 0.9800 . ? C51 H38 0.9800 . ? C51 H39 0.9800 . ? C52 H40 0.9800 . ? C52 H41 0.9800 . ? C52 H42 0.9800 . ? C102 C103 1.481(11) . ? C102 H43 0.9900 . ? C102 H44 0.9900 . ? C103 H45 0.9900 . ? C103 H46 0.9900 . ? C202 C203 1.503(11) . ? C202 H47 0.9900 . ? C202 H48 0.9900 . ? C203 H49 0.9900 . ? C203 H50 0.9900 . ? C302 C303 1.499(12) . ? C302 H51 0.9900 . ? C302 H52 0.9900 . ? C303 H53 0.9900 . ? C303 H54 0.9900 . ? C402 C403 1.498(10) . ? C402 H55 0.9900 . ? C402 H56 0.9900 . ? C403 H57 0.9900 . ? C403 H58 0.9900 . ? 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 O51 Cu1 O52 77.7(2) . . ? O51 Cu1 N201 170.0(2) . . ? O52 Cu1 N201 94.8(2) . . ? O51 Cu1 N101 94.6(2) . . ? O52 Cu1 N101 170.9(2) . . ? N201 Cu1 N101 92.3(3) . . ? O51 Cu1 O11 95.37(19) . . ? O52 Cu1 O11 91.8(2) . . ? N201 Cu1 O11 91.4(2) . . ? N101 Cu1 O11 93.6(2) . . ? O51 Cu1 Cu2 40.77(14) . . ? O52 Cu1 Cu2 40.90(14) . . ? N201 Cu1 Cu2 133.97(18) . . ? N101 Cu1 Cu2 133.17(19) . . ? O11 Cu1 Cu2 80.92(13) . . ? O51 Cu2 O52 77.6(2) . . ? O51 Cu2 N401 94.7(2) . . ? O52 Cu2 N401 171.2(2) . . ? O51 Cu2 N301 170.8(2) . . ? O52 Cu2 N301 95.2(2) . . ? N401 Cu2 N301 92.0(3) . . ? O51 Cu2 O12 94.1(2) . . ? O52 Cu2 O12 92.3(2) . . ? N401 Cu2 O12 92.6(2) . . ? N301 Cu2 O12 91.9(2) . . ? O51 Cu2 Cu1 40.75(14) . . ? O52 Cu2 Cu1 40.83(14) . . ? N401 Cu2 Cu1 133.22(17) . . ? N301 Cu2 Cu1 134.09(19) . . ? O12 Cu2 Cu1 80.40(14) . . ? O62 Cu3 O61 81.5(2) . . ? O62 Cu3 N1 174.2(2) . . ? O61 Cu3 N1 94.6(2) . . ? O62 Cu3 N2 99.0(2) . . ? O61 Cu3 N2 175.8(2) . . ? N1 Cu3 N2 84.6(2) . . ? O62 Cu3 O21 97.6(2) . . ? O61 Cu3 O21 95.4(2) . . ? N1 Cu3 O21 87.0(2) . . ? N2 Cu3 O21 88.7(2) . . ? O62 Cu3 Cu4 42.99(14) . . ? O61 Cu3 Cu4 42.76(14) . . ? N1 Cu3 Cu4 134.72(18) . . ? N2 Cu3 Cu4 139.13(18) . . ? O21 Cu3 Cu4 83.83(14) . . ? O61 Cu4 O62 81.4(2) . . ? O61 Cu4 N4 94.3(2) . . ? O62 Cu4 N4 175.3(2) . . ? O61 Cu4 N3 174.0(2) . . ? O62 Cu4 N3 99.3(2) . . ? N4 Cu4 N3 84.8(2) . . ? O61 Cu4 O22 95.8(2) . . ? O62 Cu4 O22 92.1(2) . . ? N4 Cu4 O22 90.2(2) . . ? N3 Cu4 O22 90.1(2) . . ? O61 Cu4 Cu3 42.89(14) . . ? O62 Cu4 Cu3 42.82(14) . . ? N4 Cu4 Cu3 133.77(18) . . ? N3 Cu4 Cu3 139.79(17) . . ? O22 Cu4 Cu3 80.49(14) . . ? N01 O12 Cu2 129.9(4) . . ? N01 O11 Cu1 126.9(4) . . ? N02 O21 Cu3 117.9(5) . . ? N02 O22 Cu4 124.7(4) . . ? O71 O43B N04B 163(3) . . ? C51 O51 Cu1 123.1(4) . . ? C51 O51 Cu2 121.8(4) . . ? Cu1 O51 Cu2 98.5(2) . . ? C52 O52 Cu1 123.0(5) . . ? C52 O52 Cu2 122.4(5) . . ? Cu1 O52 Cu2 98.3(2) . . ? Cu4 O61 Cu3 94.3(2) . . ? Cu3 O62 Cu4 94.2(2) . . ? O43B O71 O43B 179.992(5) 3_666 . ? C101 O101 C102 107.4(6) . . ? C201 O201 C202 106.8(6) . . ? C301 O301 C302 107.6(6) . . ? C401 O401 C402 106.9(5) . . ? C1 N1 C10 115.3(6) . . ? C1 N1 Cu3 109.7(5) . . ? C10 N1 Cu3 117.1(5) . . ? C1 N1 H1 104.4 . . ? C10 N1 H1 104.4 . . ? Cu3 N1 H1 104.4 . . ? O13 N01 O12 119.9(6) . . ? O13 N01 O11 118.3(6) . . ? O12 N01 O11 121.8(6) . . ? C20 N2 C2 110.3(6) . . ? C20 N2 Cu3 123.3(5) . . ? C2 N2 Cu3 105.8(5) . . ? C20 N2 H2 105.4 . . ? C2 N2 H2 105.4 . . ? Cu3 N2 H2 105.4 . . ? O32 N03 O33 121.5(9) . . ? O32 N03 O31 117.6(8) . . ? O33 N03 O31 120.9(8) . . ? C3 N3 C30 112.3(6) . . ? C3 N3 Cu4 106.9(4) . . ? C30 N3 Cu4 122.9(5) . . ? C3 N3 H3 104.3 . . ? C30 N3 H3 104.3 . . ? Cu4 N3 H3 104.3 . . ? O23 N02 O21 119.7(7) . . ? O23 N02 O22 118.7(7) . . ? O21 N02 O22 121.3(6) . . ? C4 N4 C40 114.1(6) . . ? C4 N4 Cu4 108.4(5) . . ? C40 N4 Cu4 118.1(4) . . ? C4 N4 H4 105.0 . . ? C40 N4 H4 105.0 . . ? Cu4 N4 H4 105.0 . . ? O41 N04 O43 118.7(7) . . ? O41 N04 O42 121.0(7) . . ? O43 N04 O42 119.5(6) . . ? O42 N04B O43B 120.8(7) . . ? O42 N04B O41B 119.2(7) . . ? O43B N04B O41B 120.0(7) . . ? C101 N101 C103 106.3(6) . . ? C101 N101 Cu1 137.0(5) . . ? C103 N101 Cu1 116.6(5) . . ? C201 N201 C203 107.0(6) . . ? C201 N201 Cu1 129.9(5) . . ? C203 N201 Cu1 123.0(5) . . ? C301 N301 C303 107.4(6) . . ? C301 N301 Cu2 133.1(5) . . ? C303 N301 Cu2 119.4(5) . . ? C401 N401 C403 107.5(6) . . ? C401 N401 Cu2 135.1(5) . . ? C403 N401 Cu2 117.4(4) . . ? C2 C1 N1 109.8(7) . . ? C2 C1 H5 109.7 . . ? N1 C1 H5 109.7 . . ? C2 C1 H6 109.7 . . ? N1 C1 H6 109.7 . . ? H5 C1 H6 108.2 . . ? C1 C2 N2 109.6(7) . . ? C1 C2 H7 109.8 . . ? N2 C2 H7 109.8 . . ? C1 C2 H8 109.8 . . ? N2 C2 H8 109.8 . . ? H7 C2 H8 108.2 . . ? N3 C3 C4 106.6(6) . . ? N3 C3 H9 110.4 . . ? C4 C3 H9 110.4 . . ? N3 C3 H10 110.4 . . ? C4 C3 H10 110.4 . . ? H9 C3 H10 108.6 . . ? N4 C4 C3 110.1(6) . . ? N4 C4 H11 109.6 . . ? C3 C4 H11 109.6 . . ? N4 C4 H12 109.6 . . ? C3 C4 H12 109.6 . . ? H11 C4 H12 108.2 . . ? N1 C10 C11 114.9(6) . . ? N1 C10 H13 108.6 . . ? C11 C10 H13 108.6 . . ? N1 C10 H14 108.6 . . ? C11 C10 H14 108.6 . . ? H13 C10 H14 107.5 . . ? C12 C11 C16 118.0(7) . . ? C12 C11 C10 121.0(7) . . ? C16 C11 C10 120.6(7) . . ? C11 C12 C13 121.5(7) . . ? C11 C12 H15 119.2 . . ? C13 C12 H15 119.2 . . ? C14 C13 C12 119.9(7) . . ? C14 C13 H16 120.0 . . ? C12 C13 H16 120.0 . . ? C13 C14 C15 119.0(7) . . ? C13 C14 C101 118.6(7) . . ? C15 C14 C101 122.3(7) . . ? C16 C15 C14 120.7(7) . . ? C16 C15 H17 119.6 . . ? C14 C15 H17 119.6 . . ? C15 C16 C11 120.9(7) . . ? C15 C16 H18 119.6 . . ? C11 C16 H18 119.6 . . ? N2 C20 C21 114.6(6) . . ? N2 C20 H19 108.6 . . ? C21 C20 H19 108.6 . . ? N2 C20 H20 108.6 . . ? C21 C20 H20 108.6 . . ? H19 C20 H20 107.6 . . ? C26 C21 C22 118.0(7) . . ? C26 C21 C20 121.2(7) . . ? C22 C21 C20 120.7(7) . . ? C23 C22 C21 120.6(7) . . ? C23 C22 H21 119.7 . . ? C21 C22 H21 119.7 . . ? C22 C23 C24 121.3(7) . . ? C22 C23 H22 119.3 . . ? C24 C23 H22 119.3 . . ? C23 C24 C25 118.5(7) . . ? C23 C24 C201 121.0(7) . . ? C25 C24 C201 120.2(7) . . ? C26 C25 C24 119.6(7) . . ? C26 C25 H23 120.2 . . ? C24 C25 H23 120.2 . . ? C25 C26 C21 121.9(7) . . ? C25 C26 H24 119.1 . . ? C21 C26 H24 119.1 . . ? N3 C30 C31 113.1(6) . . ? N3 C30 H25 109.0 . . ? C31 C30 H25 109.0 . . ? N3 C30 H26 109.0 . . ? C31 C30 H26 109.0 . . ? H25 C30 H26 107.8 . . ? C36 C31 C32 118.4(7) . . ? C36 C31 C30 120.6(7) . . ? C32 C31 C30 120.9(7) . . ? C33 C32 C31 121.6(7) . . ? C33 C32 H27 119.2 . . ? C31 C32 H27 119.2 . . ? C32 C33 C34 120.2(7) . . ? C32 C33 H28 119.9 . . ? C34 C33 H28 119.9 . . ? C33 C34 C35 118.3(7) . . ? C33 C34 C301 120.2(7) . . ? C35 C34 C301 121.3(7) . . ? C36 C35 C34 120.3(7) . . ? C36 C35 H29 119.8 . . ? C34 C35 H29 119.8 . . ? C35 C36 C31 121.0(7) . . ? C35 C36 H30 119.5 . . ? C31 C36 H30 119.5 . . ? N4 C40 C41 115.6(6) . . ? N4 C40 H31 108.4 . . ? C41 C40 H31 108.4 . . ? N4 C40 H32 108.4 . . ? C41 C40 H32 108.4 . . ? H31 C40 H32 107.4 . . ? C42 C41 C46 118.4(6) . . ? C42 C41 C40 120.1(6) . . ? C46 C41 C40 121.2(7) . . ? C43 C42 C41 121.3(7) . . ? C43 C42 H33 119.4 . . ? C41 C42 H33 119.4 . . ? C42 C43 C44 119.7(7) . . ? C42 C43 H34 120.2 . . ? C44 C43 H34 120.2 . . ? C45 C44 C43 119.2(6) . . ? C45 C44 C401 120.8(6) . . ? C43 C44 C401 119.7(6) . . ? C46 C45 C44 120.2(7) . . ? C46 C45 H35 119.9 . . ? C44 C45 H35 119.9 . . ? C45 C46 C41 121.1(7) . . ? C45 C46 H36 119.4 . . ? C41 C46 H36 119.4 . . ? O51 C51 H37 109.5 . . ? O51 C51 H38 109.5 . . ? H37 C51 H38 109.5 . . ? O51 C51 H39 109.5 . . ? H37 C51 H39 109.5 . . ? H38 C51 H39 109.5 . . ? O52 C52 H40 109.5 . . ? O52 C52 H41 109.5 . . ? H40 C52 H41 109.5 . . ? O52 C52 H42 109.5 . . ? H40 C52 H42 109.5 . . ? H41 C52 H42 109.5 . . ? N101 C101 O101 116.9(7) . . ? N101 C101 C14 127.3(7) . . ? O101 C101 C14 115.7(7) . . ? O101 C102 C103 104.5(7) . . ? O101 C102 H43 110.8 . . ? C103 C102 H43 110.8 . . ? O101 C102 H44 110.8 . . ? C103 C102 H44 110.8 . . ? H43 C102 H44 108.9 . . ? C102 C103 N101 104.8(7) . . ? C102 C103 H45 110.8 . . ? N101 C103 H45 110.8 . . ? C102 C103 H46 110.8 . . ? N101 C103 H46 110.8 . . ? H45 C103 H46 108.9 . . ? N201 C201 O201 117.4(7) . . ? N201 C201 C24 128.6(7) . . ? O201 C201 C24 114.0(6) . . ? O201 C202 C203 104.4(6) . . ? O201 C202 H47 110.9 . . ? C203 C202 H47 110.9 . . ? O201 C202 H48 110.9 . . ? C203 C202 H48 110.9 . . ? H47 C202 H48 108.9 . . ? N201 C203 C202 104.0(6) . . ? N201 C203 H49 111.0 . . ? C202 C203 H49 111.0 . . ? N201 C203 H50 111.0 . . ? C202 C203 H50 111.0 . . ? H49 C203 H50 109.0 . . ? N301 C301 O301 116.7(7) . . ? N301 C301 C34 127.6(7) . . ? O301 C301 C34 115.7(7) . . ? O301 C302 C303 104.2(6) . . ? O301 C302 H51 110.9 . . ? C303 C302 H51 110.9 . . ? O301 C302 H52 110.9 . . ? C303 C302 H52 110.9 . . ? H51 C302 H52 108.9 . . ? N301 C303 C302 104.0(7) . . ? N301 C303 H53 111.0 . . ? C302 C303 H53 111.0 . . ? N301 C303 H54 111.0 . . ? C302 C303 H54 111.0 . . ? H53 C303 H54 109.0 . . ? N401 C401 O401 116.7(6) . . ? N401 C401 C44 128.9(6) . . ? O401 C401 C44 114.3(6) . . ? O401 C402 C403 104.3(6) . . ? O401 C402 H55 110.9 . . ? C403 C402 H55 110.9 . . ? O401 C402 H56 110.9 . . ? C403 C402 H56 110.9 . . ? H55 C402 H56 108.9 . . ? N401 C403 C402 103.6(6) . . ? N401 C403 H57 111.0 . . ? C402 C403 H57 111.0 . . ? N401 C403 H58 111.0 . . ? C402 C403 H58 111.0 . . ? H57 C403 H58 109.0 . . ? 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 O52 Cu1 Cu2 O51 147.2(3) . . . . ? N201 Cu1 Cu2 O51 167.6(3) . . . . ? N101 Cu1 Cu2 O51 -22.9(3) . . . . ? O11 Cu1 Cu2 O51 -109.3(3) . . . . ? O51 Cu1 Cu2 O52 -147.2(3) . . . . ? N201 Cu1 Cu2 O52 20.4(3) . . . . ? N101 Cu1 Cu2 O52 -170.1(3) . . . . ? O11 Cu1 Cu2 O52 103.5(3) . . . . ? O51 Cu1 Cu2 N401 23.4(3) . . . . ? O52 Cu1 Cu2 N401 170.6(3) . . . . ? N201 Cu1 Cu2 N401 -169.0(3) . . . . ? N101 Cu1 Cu2 N401 0.5(3) . . . . ? O11 Cu1 Cu2 N401 -85.9(3) . . . . ? O51 Cu1 Cu2 N301 -168.8(3) . . . . ? O52 Cu1 Cu2 N301 -21.6(3) . . . . ? N201 Cu1 Cu2 N301 -1.2(4) . . . . ? N101 Cu1 Cu2 N301 168.3(3) . . . . ? O11 Cu1 Cu2 N301 81.9(3) . . . . ? O51 Cu1 Cu2 O12 107.9(3) . . . . ? O52 Cu1 Cu2 O12 -104.9(3) . . . . ? N201 Cu1 Cu2 O12 -84.5(3) . . . . ? N101 Cu1 Cu2 O12 85.0(3) . . . . ? O11 Cu1 Cu2 O12 -1.4(2) . . . . ? O62 Cu3 Cu4 O61 -147.1(3) . . . . ? N1 Cu3 Cu4 O61 25.3(3) . . . . ? N2 Cu3 Cu4 O61 -174.3(3) . . . . ? O21 Cu3 Cu4 O61 104.8(3) . . . . ? O61 Cu3 Cu4 O62 147.1(3) . . . . ? N1 Cu3 Cu4 O62 172.4(3) . . . . ? N2 Cu3 Cu4 O62 -27.2(3) . . . . ? O21 Cu3 Cu4 O62 -108.1(3) . . . . ? O62 Cu3 Cu4 N4 -175.5(3) . . . . ? O61 Cu3 Cu4 N4 -28.4(3) . . . . ? N1 Cu3 Cu4 N4 -3.0(3) . . . . ? N2 Cu3 Cu4 N4 157.3(3) . . . . ? O21 Cu3 Cu4 N4 76.5(3) . . . . ? O62 Cu3 Cu4 N3 24.8(3) . . . . ? O61 Cu3 Cu4 N3 171.9(3) . . . . ? N1 Cu3 Cu4 N3 -162.8(4) . . . . ? N2 Cu3 Cu4 N3 -2.5(4) . . . . ? O21 Cu3 Cu4 N3 -83.3(3) . . . . ? O62 Cu3 Cu4 O22 103.5(3) . . . . ? O61 Cu3 Cu4 O22 -109.4(3) . . . . ? N1 Cu3 Cu4 O22 -84.0(3) . . . . ? N2 Cu3 Cu4 O22 76.3(3) . . . . ? O21 Cu3 Cu4 O22 -4.5(2) . . . . ? O51 Cu2 O12 N01 40.7(7) . . . . ? O52 Cu2 O12 N01 -37.0(7) . . . . ? N401 Cu2 O12 N01 135.6(7) . . . . ? N301 Cu2 O12 N01 -132.3(7) . . . . ? Cu1 Cu2 O12 N01 2.2(6) . . . . ? O51 Cu1 O11 N01 -36.2(6) . . . . ? O52 Cu1 O11 N01 41.6(6) . . . . ? N201 Cu1 O11 N01 136.4(6) . . . . ? N101 Cu1 O11 N01 -131.1(6) . . . . ? Cu2 Cu1 O11 N01 2.1(6) . . . . ? O62 Cu3 O21 N02 -16.6(6) . . . . ? O61 Cu3 O21 N02 65.5(6) . . . . ? N1 Cu3 O21 N02 159.8(6) . . . . ? N2 Cu3 O21 N02 -115.5(6) . . . . ? Cu4 Cu3 O21 N02 24.2(5) . . . . ? O61 Cu4 O22 N02 -52.9(7) . . . . ? O62 Cu4 O22 N02 28.7(7) . . . . ? N4 Cu4 O22 N02 -147.2(7) . . . . ? N3 Cu4 O22 N02 128.0(7) . . . . ? Cu3 Cu4 O22 N02 -12.7(7) . . . . ? O52 Cu1 O51 C51 -158.4(6) . . . . ? N101 Cu1 O51 C51 26.3(6) . . . . ? O11 Cu1 O51 C51 -67.7(5) . . . . ? Cu2 Cu1 O51 C51 -137.1(6) . . . . ? O52 Cu1 O51 Cu2 -21.3(2) . . . . ? N101 Cu1 O51 Cu2 163.5(2) . . . . ? O11 Cu1 O51 Cu2 69.4(2) . . . . ? O52 Cu2 O51 C51 159.1(5) . . . . ? N401 Cu2 O51 C51 -25.2(5) . . . . ? O12 Cu2 O51 C51 67.7(5) . . . . ? Cu1 Cu2 O51 C51 137.9(6) . . . . ? O52 Cu2 O51 Cu1 21.26(19) . . . . ? N401 Cu2 O51 Cu1 -163.1(2) . . . . ? O12 Cu2 O51 Cu1 -70.2(2) . . . . ? O51 Cu1 O52 C52 158.9(6) . . . . ? N201 Cu1 O52 C52 -27.7(6) . . . . ? O11 Cu1 O52 C52 63.8(6) . . . . ? Cu2 Cu1 O52 C52 137.7(7) . . . . ? O51 Cu1 O52 Cu2 21.23(19) . . . . ? N201 Cu1 O52 Cu2 -165.4(2) . . . . ? O11 Cu1 O52 Cu2 -73.9(2) . . . . ? O51 Cu2 O52 C52 -159.3(6) . . . . ? N301 Cu2 O52 C52 26.5(6) . . . . ? O12 Cu2 O52 C52 -65.6(6) . . . . ? Cu1 Cu2 O52 C52 -138.1(6) . . . . ? O51 Cu2 O52 Cu1 -21.23(19) . . . . ? N301 Cu2 O52 Cu1 164.6(2) . . . . ? O12 Cu2 O52 Cu1 72.5(2) . . . . ? O62 Cu4 O61 Cu3 -21.9(2) . . . . ? N4 Cu4 O61 Cu3 159.9(2) . . . . ? O22 Cu4 O61 Cu3 69.3(2) . . . . ? O62 Cu3 O61 Cu4 22.0(2) . . . . ? N1 Cu3 O61 Cu4 -162.3(2) . . . . ? O21 Cu3 O61 Cu4 -74.9(2) . . . . ? O61 Cu3 O62 Cu4 -21.9(2) . . . . ? N2 Cu3 O62 Cu4 162.3(2) . . . . ? O21 Cu3 O62 Cu4 72.4(2) . . . . ? O61 Cu4 O62 Cu3 22.0(2) . . . . ? N3 Cu4 O62 Cu3 -164.1(2) . . . . ? O22 Cu4 O62 Cu3 -73.6(2) . . . . ? O61 Cu3 N1 C1 178.6(6) . . . . ? N2 Cu3 N1 C1 -5.5(6) . . . . ? O21 Cu3 N1 C1 83.5(6) . . . . ? Cu4 Cu3 N1 C1 161.7(5) . . . . ? O61 Cu3 N1 C10 -47.5(5) . . . . ? N2 Cu3 N1 C10 128.4(5) . . . . ? O21 Cu3 N1 C10 -142.6(5) . . . . ? Cu4 Cu3 N1 C10 -64.4(6) . . . . ? Cu2 O12 N01 O13 177.1(6) . . . . ? Cu2 O12 N01 O11 -1.3(11) . . . . ? Cu1 O11 N01 O13 -179.6(5) . . . . ? Cu1 O11 N01 O12 -1.1(10) . . . . ? O62 Cu3 N2 C20 27.5(6) . . . . ? N1 Cu3 N2 C20 -147.9(6) . . . . ? O21 Cu3 N2 C20 125.0(6) . . . . ? Cu4 Cu3 N2 C20 46.0(7) . . . . ? O62 Cu3 N2 C2 155.6(5) . . . . ? N1 Cu3 N2 C2 -19.9(5) . . . . ? O21 Cu3 N2 C2 -107.0(5) . . . . ? Cu4 Cu3 N2 C2 174.0(4) . . . . ? O62 Cu4 N3 C3 -156.3(4) . . . . ? N4 Cu4 N3 C3 21.4(4) . . . . ? O22 Cu4 N3 C3 111.6(4) . . . . ? Cu3 Cu4 N3 C3 -173.1(3) . . . . ? O62 Cu4 N3 C30 -24.2(5) . . . . ? N4 Cu4 N3 C30 153.5(5) . . . . ? O22 Cu4 N3 C30 -116.3(5) . . . . ? Cu3 Cu4 N3 C30 -41.0(6) . . . . ? Cu3 O21 N02 O23 143.2(6) . . . . ? Cu3 O21 N02 O22 -42.3(9) . . . . ? Cu4 O22 N02 O23 -147.7(6) . . . . ? Cu4 O22 N02 O21 37.8(10) . . . . ? O61 Cu4 N4 C4 -179.2(4) . . . . ? N3 Cu4 N4 C4 6.8(4) . . . . ? O22 Cu4 N4 C4 -83.3(5) . . . . ? Cu3 Cu4 N4 C4 -160.3(4) . . . . ? O61 Cu4 N4 C40 49.1(5) . . . . ? N3 Cu4 N4 C40 -124.9(5) . . . . ? O22 Cu4 N4 C40 145.0(5) . . . . ? Cu3 Cu4 N4 C40 68.0(5) . . . . ? O71 O43B N04B O41B 115(6) . . . . ? O51 Cu1 N101 C101 76.2(8) . . . . ? N201 Cu1 N101 C101 -96.5(8) . . . . ? O11 Cu1 N101 C101 171.9(8) . . . . ? Cu2 Cu1 N101 C101 91.0(8) . . . . ? O51 Cu1 N101 C103 -105.0(6) . . . . ? N201 Cu1 N101 C103 82.2(6) . . . . ? O11 Cu1 N101 C103 -9.4(6) . . . . ? Cu2 Cu1 N101 C103 -90.3(6) . . . . ? O52 Cu1 N201 C201 -87.5(7) . . . . ? N101 Cu1 N201 C201 86.9(7) . . . . ? O11 Cu1 N201 C201 -179.5(7) . . . . ? Cu2 Cu1 N201 C201 -100.8(7) . . . . ? O52 Cu1 N201 C203 96.1(6) . . . . ? N101 Cu1 N201 C203 -89.5(6) . . . . ? O11 Cu1 N201 C203 4.2(6) . . . . ? Cu2 Cu1 N201 C203 82.9(6) . . . . ? O52 Cu2 N301 C301 81.7(8) . . . . ? N401 Cu2 N301 C301 -93.2(8) . . . . ? O12 Cu2 N301 C301 174.2(8) . . . . ? Cu1 Cu2 N301 C301 95.7(7) . . . . ? O52 Cu2 N301 C303 -100.9(6) . . . . ? N401 Cu2 N301 C303 84.2(6) . . . . ? O12 Cu2 N301 C303 -8.4(6) . . . . ? Cu1 Cu2 N301 C303 -86.9(6) . . . . ? O51 Cu2 N401 C401 -85.4(7) . . . . ? N301 Cu2 N401 C401 88.2(7) . . . . ? O12 Cu2 N401 C401 -179.8(7) . . . . ? Cu1 Cu2 N401 C401 -100.5(7) . . . . ? O51 Cu2 N401 C403 97.6(5) . . . . ? N301 Cu2 N401 C403 -88.8(5) . . . . ? O12 Cu2 N401 C403 3.2(5) . . . . ? Cu1 Cu2 N401 C403 82.5(5) . . . . ? C10 N1 C1 C2 -103.2(8) . . . . ? Cu3 N1 C1 C2 31.6(9) . . . . ? N1 C1 C2 N2 -50.1(10) . . . . ? C20 N2 C2 C1 178.6(7) . . . . ? Cu3 N2 C2 C1 43.2(8) . . . . ? C30 N3 C3 C4 177.7(6) . . . . ? Cu4 N3 C3 C4 -44.6(6) . . . . ? C40 N4 C4 C3 99.7(7) . . . . ? Cu4 N4 C4 C3 -34.0(7) . . . . ? N3 C3 C4 N4 52.9(8) . . . . ? C1 N1 C10 C11 72.4(9) . . . . ? Cu3 N1 C10 C11 -59.0(8) . . . . ? N1 C10 C11 C12 -112.2(9) . . . . ? N1 C10 C11 C16 75.7(9) . . . . ? C16 C11 C12 C13 0.5(13) . . . . ? C10 C11 C12 C13 -171.8(8) . . . . ? C11 C12 C13 C14 0.9(14) . . . . ? C12 C13 C14 C15 -2.7(13) . . . . ? C12 C13 C14 C101 172.9(8) . . . . ? C13 C14 C15 C16 3.2(12) . . . . ? C101 C14 C15 C16 -172.2(7) . . . . ? C14 C15 C16 C11 -1.8(12) . . . . ? C12 C11 C16 C15 -0.1(12) . . . . ? C10 C11 C16 C15 172.2(7) . . . . ? C2 N2 C20 C21 -59.5(8) . . . . ? Cu3 N2 C20 C21 66.6(8) . . . . ? N2 C20 C21 C26 -81.3(9) . . . . ? N2 C20 C21 C22 102.1(8) . . . . ? C26 C21 C22 C23 -3.3(12) . . . . ? C20 C21 C22 C23 173.4(7) . . . . ? C21 C22 C23 C24 1.8(13) . . . . ? C22 C23 C24 C25 0.3(12) . . . . ? C22 C23 C24 C201 -174.2(8) . . . . ? C23 C24 C25 C26 -0.7(12) . . . . ? C201 C24 C25 C26 173.8(7) . . . . ? C24 C25 C26 C21 -0.9(13) . . . . ? C22 C21 C26 C25 2.9(12) . . . . ? C20 C21 C26 C25 -173.8(7) . . . . ? C3 N3 C30 C31 57.5(8) . . . . ? Cu4 N3 C30 C31 -72.4(7) . . . . ? N3 C30 C31 C36 75.2(9) . . . . ? N3 C30 C31 C32 -107.8(8) . . . . ? C36 C31 C32 C33 -0.2(12) . . . . ? C30 C31 C32 C33 -177.3(8) . . . . ? C31 C32 C33 C34 -0.7(13) . . . . ? C32 C33 C34 C35 1.2(12) . . . . ? C32 C33 C34 C301 177.5(8) . . . . ? C33 C34 C35 C36 -0.9(12) . . . . ? C301 C34 C35 C36 -177.1(7) . . . . ? C34 C35 C36 C31 0.0(12) . . . . ? C32 C31 C36 C35 0.6(12) . . . . ? C30 C31 C36 C35 177.6(7) . . . . ? C4 N4 C40 C41 -76.5(8) . . . . ? Cu4 N4 C40 C41 52.5(8) . . . . ? N4 C40 C41 C42 110.9(8) . . . . ? N4 C40 C41 C46 -76.1(9) . . . . ? C46 C41 C42 C43 -2.8(11) . . . . ? C40 C41 C42 C43 170.4(7) . . . . ? C41 C42 C43 C44 0.8(12) . . . . ? C42 C43 C44 C45 2.2(11) . . . . ? C42 C43 C44 C401 -171.3(7) . . . . ? C43 C44 C45 C46 -3.0(12) . . . . ? C401 C44 C45 C46 170.3(7) . . . . ? C44 C45 C46 C41 1.0(12) . . . . ? C42 C41 C46 C45 1.9(11) . . . . ? C40 C41 C46 C45 -171.2(7) . . . . ? C103 N101 C101 O101 -2.3(10) . . . . ? Cu1 N101 C101 O101 176.5(6) . . . . ? C103 N101 C101 C14 174.5(8) . . . . ? Cu1 N101 C101 C14 -6.7(14) . . . . ? C102 O101 C101 N101 2.5(11) . . . . ? C102 O101 C101 C14 -174.7(8) . . . . ? C13 C14 C101 N101 164.4(8) . . . . ? C15 C14 C101 N101 -20.1(13) . . . . ? C13 C14 C101 O101 -18.7(11) . . . . ? C15 C14 C101 O101 156.7(8) . . . . ? C101 O101 C102 C103 -1.5(11) . . . . ? O101 C102 C103 N101 0.2(11) . . . . ? C101 N101 C103 C102 1.1(10) . . . . ? Cu1 N101 C103 C102 -178.0(7) . . . . ? C203 N201 C201 O201 2.6(9) . . . . ? Cu1 N201 C201 O201 -174.2(5) . . . . ? C203 N201 C201 C24 -176.3(8) . . . . ? Cu1 N201 C201 C24 6.9(12) . . . . ? C202 O201 C201 N201 1.4(9) . . . . ? C202 O201 C201 C24 -179.5(6) . . . . ? C23 C24 C201 N201 -150.4(8) . . . . ? C25 C24 C201 N201 35.2(12) . . . . ? C23 C24 C201 O201 30.6(11) . . . . ? C25 C24 C201 O201 -143.8(7) . . . . ? C201 O201 C202 C203 -4.6(9) . . . . ? C201 N201 C203 C202 -5.3(9) . . . . ? Cu1 N201 C203 C202 171.8(5) . . . . ? O201 C202 C203 N201 5.8(8) . . . . ? C303 N301 C301 O301 -2.2(10) . . . . ? Cu2 N301 C301 O301 175.4(5) . . . . ? C303 N301 C301 C34 176.7(8) . . . . ? Cu2 N301 C301 C34 -5.7(13) . . . . ? C302 O301 C301 N301 0.3(10) . . . . ? C302 O301 C301 C34 -178.7(7) . . . . ? C33 C34 C301 N301 163.0(8) . . . . ? C35 C34 C301 N301 -20.9(13) . . . . ? C33 C34 C301 O301 -18.2(11) . . . . ? C35 C34 C301 O301 158.0(7) . . . . ? C301 O301 C302 C303 1.6(10) . . . . ? C301 N301 C303 C302 3.0(10) . . . . ? Cu2 N301 C303 C302 -175.0(6) . . . . ? O301 C302 C303 N301 -2.7(10) . . . . ? C403 N401 C401 O401 3.9(9) . . . . ? Cu2 N401 C401 O401 -173.3(5) . . . . ? C403 N401 C401 C44 -171.6(7) . . . . ? Cu2 N401 C401 C44 11.2(12) . . . . ? C402 O401 C401 N401 2.8(9) . . . . ? C402 O401 C401 C44 179.0(6) . . . . ? C45 C44 C401 N401 29.1(12) . . . . ? C43 C44 C401 N401 -157.6(8) . . . . ? C45 C44 C401 O401 -146.5(7) . . . . ? C43 C44 C401 O401 26.8(10) . . . . ? C401 O401 C402 C403 -8.0(8) . . . . ? C401 N401 C403 C402 -8.6(8) . . . . ? Cu2 N401 C403 C402 169.1(5) . . . . ? O401 C402 C403 N401 9.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.851 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.132 #====END