# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Dong-Bin Dang' _publ_contact_author_email DANGDB@HENU.EDU.CN _publ_section_title ; A series of metal-organic frameworks based on polydentate Schiff-base ligands derived from benzil dihydrazone: synthesis, crystal structures and luminescent properties ; loop_ _publ_author_name 'Dong-Bin Dang' 'Bing An' 'Yan Bai' 'Hui Gao' 'Xiang-Yang Guo' ; Wei-Li Shang ; # Attachment 'cif.cif' # Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_1 _database_code_depnum_ccdc_archive 'CCDC 748790' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Ag N6, Cl O4' _chemical_formula_sum 'C26 H20 Ag Cl N6 O4' _chemical_formula_weight 623.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.7617(2) _cell_length_b 16.4570(2) _cell_length_c 19.1902(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5293.56(11) _cell_formula_units_Z 8 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 8128 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27128 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4930 _reflns_number_gt 3835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+4.2659P] 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 4930 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 0.136098(13) 0.742887(13) 0.251340(11) 0.04206(9) Uani 1 1 d . . . N1 N 0.45573(14) 0.33784(13) 0.24133(11) 0.0388(5) Uani 1 1 d . . . N2 N 0.62239(12) 0.57238(12) 0.15356(11) 0.0353(5) Uani 1 1 d . . . N3 N 0.64655(12) 0.65457(12) 0.15121(11) 0.0323(5) Uani 1 1 d . . . N4 N 0.55060(13) 0.62146(14) 0.01131(11) 0.0398(5) Uani 1 1 d . . . N5 N 0.49834(13) 0.64890(15) 0.06329(11) 0.0429(5) Uani 1 1 d . . . N6 N 0.23830(13) 0.70729(16) 0.18347(12) 0.0495(6) Uani 1 1 d . . . C1 C 0.53681(17) 0.42118(16) 0.16852(13) 0.0423(6) Uani 1 1 d . . . H1A H 0.5623 0.4286 0.1254 0.051 Uiso 1 1 calc R . . C2 C 0.49230(18) 0.35260(16) 0.18059(14) 0.0455(7) Uani 1 1 d . . . H2A H 0.4872 0.3142 0.1446 0.055 Uiso 1 1 calc R . . C3 C 0.46500(18) 0.39280(18) 0.29141(14) 0.0478(7) Uani 1 1 d . . . H3A H 0.4408 0.3828 0.3348 0.057 Uiso 1 1 calc R . . C4 C 0.50776(17) 0.46321(18) 0.28348(14) 0.0458(7) Uani 1 1 d . . . H4A H 0.5125 0.5002 0.3205 0.055 Uiso 1 1 calc R . . C5 C 0.54386(15) 0.47889(15) 0.21999(13) 0.0340(5) Uani 1 1 d . . . C6 C 0.58396(15) 0.55695(15) 0.20912(13) 0.0361(6) Uani 1 1 d . . . H6A H 0.5812 0.5967 0.2442 0.043 Uiso 1 1 calc R . . C7 C 0.64742(14) 0.68461(15) 0.08938(12) 0.0304(5) Uani 1 1 d . . . C8 C 0.66614(14) 0.77242(15) 0.08247(12) 0.0320(5) Uani 1 1 d . . . C9 C 0.72739(16) 0.80699(16) 0.12121(14) 0.0400(6) Uani 1 1 d . . . H9A H 0.7607 0.7740 0.1486 0.048 Uiso 1 1 calc R . . C10 C 0.73900(18) 0.89018(18) 0.11917(16) 0.0501(7) Uani 1 1 d . . . H10A H 0.7802 0.9138 0.1455 0.060 Uiso 1 1 calc R . . C11 C 0.69047(19) 0.93874(17) 0.07878(16) 0.0523(8) Uani 1 1 d . . . H11A H 0.6982 0.9953 0.0783 0.063 Uiso 1 1 calc R . . C12 C 0.63089(17) 0.90468(17) 0.03915(15) 0.0459(7) Uani 1 1 d . . . H12A H 0.5983 0.9380 0.0113 0.055 Uiso 1 1 calc R . . C13 C 0.61873(15) 0.82123(16) 0.04012(13) 0.0362(6) Uani 1 1 d . . . H13A H 0.5787 0.7978 0.0123 0.043 Uiso 1 1 calc R . . C14 C 0.62375(15) 0.63732(15) 0.02515(13) 0.0318(5) Uani 1 1 d . . . C15 C 0.68613(15) 0.61280(15) -0.02464(13) 0.0351(6) Uani 1 1 d . . . C16 C 0.76581(17) 0.63247(18) -0.01384(15) 0.0458(7) Uani 1 1 d . . . H16A H 0.7809 0.6614 0.0263 0.055 Uiso 1 1 calc R . . C17 C 0.82300(19) 0.6096(2) -0.06216(18) 0.0628(9) Uani 1 1 d . . . H17A H 0.8769 0.6228 -0.0547 0.075 Uiso 1 1 calc R . . C18 C 0.8011(2) 0.5678(3) -0.12048(19) 0.0792(12) Uani 1 1 d . . . H18A H 0.8400 0.5530 -0.1534 0.095 Uiso 1 1 calc R . . C19 C 0.7222(2) 0.5470(3) -0.13178(18) 0.0803(12) Uani 1 1 d . . . H19A H 0.7077 0.5182 -0.1721 0.096 Uiso 1 1 calc R . . C20 C 0.66495(19) 0.5686(2) -0.08374(15) 0.0571(8) Uani 1 1 d . . . H20A H 0.6115 0.5535 -0.0908 0.069 Uiso 1 1 calc R . . C21 C 0.42642(16) 0.64077(19) 0.04730(14) 0.0452(7) Uani 1 1 d . . . H21A H 0.4131 0.6189 0.0035 0.054 Uiso 1 1 calc R . . C22 C 0.36268(15) 0.66441(19) 0.09501(14) 0.0442(7) Uani 1 1 d . . . C23 C 0.37729(18) 0.6879(3) 0.16212(17) 0.0686(11) Uani 1 1 d . . . H23A H 0.4298 0.6892 0.1793 0.082 Uiso 1 1 calc R . . C24 C 0.3148(2) 0.7094(3) 0.20387(17) 0.0776(12) Uani 1 1 d . . . H24A H 0.3260 0.7266 0.2495 0.093 Uiso 1 1 calc R . . C25 C 0.22495(17) 0.6849(2) 0.11846(15) 0.0588(9) Uani 1 1 d . . . H25A H 0.1720 0.6839 0.1023 0.071 Uiso 1 1 calc R . . C26 C 0.28457(17) 0.6630(2) 0.07351(15) 0.0608(9) Uani 1 1 d . . . H26A H 0.2720 0.6470 0.0278 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.95263(5) 0.65091(4) 0.10921(4) 0.05083(19) Uani 1 1 d . . . O1 O 1.02412(18) 0.66229(15) 0.14690(17) 0.0995(10) Uani 1 1 d . . . O2 O 0.8873(2) 0.6411(3) 0.1509(2) 0.1404(15) Uani 1 1 d . . . O3 O 0.94072(18) 0.71822(15) 0.06407(14) 0.0900(9) Uani 1 1 d . . . O4 O 0.96172(18) 0.57873(16) 0.06943(14) 0.0893(8) 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 0.03431(14) 0.04263(14) 0.04924(15) 0.00342(9) 0.00545(9) 0.00821(8) N1 0.0370(13) 0.0401(12) 0.0393(12) 0.0016(9) 0.0023(10) -0.0081(10) N2 0.0383(12) 0.0311(11) 0.0366(12) 0.0022(9) 0.0031(10) -0.0017(9) N3 0.0314(11) 0.0307(10) 0.0348(11) 0.0019(9) 0.0040(9) -0.0011(8) N4 0.0296(13) 0.0511(13) 0.0388(12) -0.0095(10) 0.0055(10) -0.0018(10) N5 0.0288(12) 0.0615(15) 0.0383(12) -0.0113(11) 0.0041(10) -0.0003(10) N6 0.0316(13) 0.0802(18) 0.0367(13) 0.0064(12) 0.0018(10) 0.0134(12) C1 0.0499(17) 0.0422(15) 0.0346(14) -0.0019(11) 0.0119(12) -0.0061(13) C2 0.0579(18) 0.0387(15) 0.0399(15) -0.0079(12) 0.0081(13) -0.0085(13) C3 0.0534(18) 0.0537(17) 0.0362(15) -0.0028(13) 0.0111(13) -0.0155(14) C4 0.0538(18) 0.0484(16) 0.0354(15) -0.0090(12) 0.0088(13) -0.0116(13) C5 0.0311(14) 0.0379(13) 0.0332(13) 0.0023(11) 0.0018(11) -0.0003(11) C6 0.0361(14) 0.0375(14) 0.0346(14) -0.0018(11) 0.0005(11) -0.0048(11) C7 0.0223(12) 0.0346(13) 0.0343(13) 0.0009(10) 0.0040(10) 0.0021(9) C8 0.0284(13) 0.0356(13) 0.0320(13) 0.0005(10) 0.0074(10) -0.0009(10) C9 0.0357(15) 0.0425(15) 0.0419(15) 0.0031(12) -0.0003(12) -0.0041(11) C10 0.0478(18) 0.0480(17) 0.0545(17) -0.0045(14) 0.0044(14) -0.0161(14) C11 0.062(2) 0.0347(15) 0.0600(19) 0.0025(13) 0.0141(16) -0.0081(14) C12 0.0498(18) 0.0407(15) 0.0473(17) 0.0101(13) 0.0143(14) 0.0085(13) C13 0.0332(14) 0.0409(14) 0.0344(14) 0.0033(11) 0.0072(11) 0.0026(11) C14 0.0302(14) 0.0328(13) 0.0323(13) 0.0026(11) 0.0039(10) 0.0021(10) C15 0.0322(14) 0.0372(13) 0.0360(13) 0.0029(11) 0.0050(11) 0.0060(11) C16 0.0338(16) 0.0566(17) 0.0470(16) -0.0005(13) 0.0059(13) 0.0038(13) C17 0.0365(17) 0.087(2) 0.065(2) -0.0013(18) 0.0158(16) 0.0062(16) C18 0.054(2) 0.120(3) 0.064(2) -0.019(2) 0.0280(19) 0.017(2) C19 0.070(3) 0.115(3) 0.056(2) -0.038(2) 0.0114(19) 0.010(2) C20 0.0419(17) 0.081(2) 0.0487(17) -0.0175(16) 0.0035(14) 0.0041(16) C21 0.0324(16) 0.0695(19) 0.0338(14) -0.0058(13) 0.0019(12) -0.0031(13) C22 0.0296(15) 0.068(2) 0.0349(14) -0.0001(13) -0.0014(11) 0.0003(12) C23 0.0284(16) 0.130(3) 0.0468(18) -0.024(2) -0.0075(13) 0.0156(18) C24 0.0412(19) 0.153(4) 0.0390(17) -0.024(2) -0.0068(15) 0.026(2) C25 0.0275(15) 0.107(3) 0.0422(17) -0.0009(17) -0.0020(13) 0.0069(16) C26 0.0298(15) 0.116(3) 0.0369(16) -0.0120(17) -0.0042(13) 0.0043(17) Cl1 0.0508(4) 0.0505(4) 0.0513(4) 0.0035(3) -0.0013(3) -0.0064(3) O1 0.101(2) 0.0600(15) 0.138(3) 0.0053(16) -0.076(2) -0.0080(14) O2 0.124(3) 0.173(4) 0.124(3) 0.020(3) 0.072(2) 0.014(3) O3 0.116(2) 0.0634(15) 0.0902(19) 0.0234(14) -0.0428(18) -0.0113(16) O4 0.115(2) 0.0615(15) 0.0909(19) -0.0184(14) -0.0108(17) -0.0072(15) _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 2.202(2) 8_665 ? Ag1 N6 2.230(2) . ? Ag1 N3 2.375(2) 6_556 ? N1 C3 1.329(3) . ? N1 C2 1.339(3) . ? N1 Ag1 2.202(2) 8_655 ? N2 C6 1.271(3) . ? N2 N3 1.413(3) . ? N3 C7 1.285(3) . ? N3 Ag1 2.375(2) 6_656 ? N4 C14 1.281(3) . ? N4 N5 1.402(3) . ? N5 C21 1.251(3) . ? N6 C25 1.320(4) . ? N6 C24 1.341(4) . ? C1 C2 1.373(4) . ? C1 C5 1.375(3) . ? C1 H1A 0.9400 . ? C2 H2A 0.9400 . ? C3 C4 1.371(4) . ? C3 H3A 0.9400 . ? C4 C5 1.385(4) . ? C4 H4A 0.9400 . ? C5 C6 1.465(3) . ? C6 H6A 0.9400 . ? C7 C8 1.485(3) . ? C7 C14 1.511(3) . ? C8 C9 1.389(3) . ? C8 C13 1.392(4) . ? C9 C10 1.383(4) . ? C9 H9A 0.9400 . ? C10 C11 1.379(4) . ? C10 H10A 0.9400 . ? C11 C12 1.375(4) . ? C11 H11A 0.9400 . ? C12 C13 1.388(4) . ? C12 H12A 0.9400 . ? C13 H13A 0.9400 . ? C14 C15 1.473(3) . ? C15 C16 1.390(4) . ? C15 C20 1.393(4) . ? C16 C17 1.386(4) . ? C16 H16A 0.9400 . ? C17 C18 1.364(5) . ? C17 H17A 0.9400 . ? C18 C19 1.382(5) . ? C18 H18A 0.9400 . ? C19 C20 1.377(4) . ? C19 H19A 0.9400 . ? C20 H20A 0.9400 . ? C21 C22 1.460(4) . ? C21 H21A 0.9400 . ? C22 C23 1.366(4) . ? C22 C26 1.373(4) . ? C23 C24 1.366(4) . ? C23 H23A 0.9400 . ? C24 H24A 0.9400 . ? C25 C26 1.368(4) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? Cl1 O2 1.366(3) . ? Cl1 O1 1.412(3) . ? Cl1 O4 1.420(3) . ? Cl1 O3 1.420(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N6 132.26(8) 8_665 . ? N1 Ag1 N3 123.68(7) 8_665 6_556 ? N6 Ag1 N3 104.03(8) . 6_556 ? C3 N1 C2 116.9(2) . . ? C3 N1 Ag1 120.11(18) . 8_655 ? C2 N1 Ag1 121.64(17) . 8_655 ? C6 N2 N3 111.3(2) . . ? C7 N3 N2 113.6(2) . . ? C7 N3 Ag1 119.49(16) . 6_656 ? N2 N3 Ag1 122.66(14) . 6_656 ? C14 N4 N5 112.6(2) . . ? C21 N5 N4 113.1(2) . . ? C25 N6 C24 116.4(3) . . ? C25 N6 Ag1 119.68(19) . . ? C24 N6 Ag1 123.9(2) . . ? C2 C1 C5 119.6(2) . . ? C2 C1 H1A 120.2 . . ? C5 C1 H1A 120.2 . . ? N1 C2 C1 123.0(2) . . ? N1 C2 H2A 118.5 . . ? C1 C2 H2A 118.5 . . ? N1 C3 C4 123.8(2) . . ? N1 C3 H3A 118.1 . . ? C4 C3 H3A 118.1 . . ? C3 C4 C5 118.9(2) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? C1 C5 C4 117.8(2) . . ? C1 C5 C6 122.9(2) . . ? C4 C5 C6 119.3(2) . . ? N2 C6 C5 121.8(2) . . ? N2 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? N3 C7 C8 117.3(2) . . ? N3 C7 C14 123.5(2) . . ? C8 C7 C14 118.9(2) . . ? C9 C8 C13 119.9(2) . . ? C9 C8 C7 120.5(2) . . ? C13 C8 C7 119.6(2) . . ? C10 C9 C8 119.6(3) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C11 C10 C9 120.4(3) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C12 C11 C10 120.2(3) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C12 C13 C8 119.7(3) . . ? C12 C13 H13A 120.2 . . ? C8 C13 H13A 120.2 . . ? N4 C14 C15 119.3(2) . . ? N4 C14 C7 121.7(2) . . ? C15 C14 C7 118.9(2) . . ? C16 C15 C20 119.2(3) . . ? C16 C15 C14 121.5(2) . . ? C20 C15 C14 119.3(2) . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C17 C18 C19 120.8(3) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C15 120.1(3) . . ? C19 C20 H20A 119.9 . . ? C15 C20 H20A 119.9 . . ? N5 C21 C22 121.5(3) . . ? N5 C21 H21A 119.2 . . ? C22 C21 H21A 119.2 . . ? C23 C22 C26 117.3(3) . . ? C23 C22 C21 122.4(3) . . ? C26 C22 C21 120.3(3) . . ? C24 C23 C22 119.2(3) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? N6 C24 C23 123.8(3) . . ? N6 C24 H24A 118.1 . . ? C23 C24 H24A 118.1 . . ? N6 C25 C26 123.1(3) . . ? N6 C25 H25A 118.5 . . ? C26 C25 H25A 118.5 . . ? C25 C26 C22 120.2(3) . . ? C25 C26 H26A 119.9 . . ? C22 C26 H26A 119.9 . . ? O2 Cl1 O1 113.3(2) . . ? O2 Cl1 O4 107.6(2) . . ? O1 Cl1 O4 107.17(18) . . ? O2 Cl1 O3 109.7(2) . . ? O1 Cl1 O3 109.16(16) . . ? O4 Cl1 O3 109.85(17) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.519 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.057 # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 748791' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H40 Ag B F4 N12' _chemical_formula_weight 1027.64 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5733(4) _cell_length_b 11.1066(4) _cell_length_c 21.3032(8) _cell_angle_alpha 98.176(2) _cell_angle_beta 93.162(2) _cell_angle_gamma 97.274(2) _cell_volume 2449.52(16) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9650 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.83 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33638 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.57 _reflns_number_total 11265 _reflns_number_gt 8278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+1.5950P] 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 11265 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.10951(2) 0.95041(3) 0.742049(11) 0.06596(10) Uani 1 1 d . . . N1 N -0.0430(2) 0.9575(2) 0.65952(11) 0.0548(6) Uani 1 1 d . . . N2 N -0.3043(2) 1.1202(2) 0.49682(12) 0.0589(6) Uani 1 1 d . . . N3 N -0.3972(3) 1.1223(2) 0.44709(11) 0.0574(6) Uani 1 1 d . . . N4 N -0.3671(2) 1.3810(2) 0.53655(10) 0.0466(5) Uani 1 1 d . . . N5 N -0.4688(2) 1.3100(2) 0.55938(10) 0.0503(5) Uani 1 1 d . . . N6 N -0.7280(2) 1.0886(2) 0.70845(11) 0.0589(6) Uani 1 1 d . . . C1 C -0.1661(3) 1.0903(3) 0.61126(14) 0.0554(7) Uani 1 1 d . . . H1 H -0.1886 1.1686 0.6115 0.066 Uiso 1 1 calc R . . C2 C -0.0813(3) 1.0673(3) 0.65754(14) 0.0599(7) Uani 1 1 d . . . H2 H -0.0484 1.1316 0.6894 0.072 Uiso 1 1 calc R . . C3 C -0.0944(3) 0.8666(3) 0.61508(15) 0.0614(8) Uani 1 1 d . . . H3 H -0.0695 0.7894 0.6157 0.074 Uiso 1 1 calc R . . C4 C -0.1834(3) 0.8806(3) 0.56771(15) 0.0624(8) Uani 1 1 d . . . H4 H -0.2199 0.8133 0.5384 0.075 Uiso 1 1 calc R . . C5 C -0.2178(3) 0.9956(2) 0.56426(13) 0.0498(6) Uani 1 1 d . . . C6 C -0.3075(3) 1.0148(3) 0.51333(14) 0.0554(7) Uani 1 1 d . . . H6 H -0.3667 0.9500 0.4931 0.067 Uiso 1 1 calc R . . C7 C -0.4149(3) 1.2310(2) 0.43919(12) 0.0434(6) Uani 1 1 d . . . C8 C -0.5093(3) 1.2448(2) 0.38808(12) 0.0449(6) Uani 1 1 d . . . C9 C -0.5465(3) 1.1488(3) 0.33834(14) 0.0611(8) Uani 1 1 d . . . H9 H -0.5105 1.0764 0.3368 0.073 Uiso 1 1 calc R . . C10 C -0.6369(4) 1.1614(3) 0.29146(15) 0.0708(9) Uani 1 1 d . . . H10 H -0.6606 1.0977 0.2579 0.085 Uiso 1 1 calc R . . C11 C -0.6922(3) 1.2674(3) 0.29390(15) 0.0626(8) Uani 1 1 d . . . H11 H -0.7533 1.2752 0.2622 0.075 Uiso 1 1 calc R . . C12 C -0.6574(3) 1.3612(3) 0.34288(15) 0.0584(7) Uani 1 1 d . . . H12 H -0.6957 1.4324 0.3448 0.070 Uiso 1 1 calc R . . C13 C -0.5654(3) 1.3507(2) 0.38975(13) 0.0495(6) Uani 1 1 d . . . H13 H -0.5411 1.4155 0.4226 0.059 Uiso 1 1 calc R . . C14 C -0.3437(2) 1.3446(2) 0.47920(11) 0.0407(5) Uani 1 1 d . . . C15 C -0.2418(3) 1.4180(2) 0.45082(12) 0.0461(6) Uani 1 1 d . . . C16 C -0.1974(4) 1.3750(4) 0.39331(15) 0.0763(10) Uani 1 1 d . . . H16 H -0.2329 1.2987 0.3713 0.092 Uiso 1 1 calc R . . C17 C -0.1008(4) 1.4442(5) 0.36828(18) 0.1022(15) Uani 1 1 d . . . H17 H -0.0722 1.4141 0.3294 0.123 Uiso 1 1 calc R . . C18 C -0.0466(4) 1.5560(4) 0.39953(19) 0.0896(12) Uani 1 1 d . . . H18 H 0.0183 1.6021 0.3820 0.108 Uiso 1 1 calc R . . C19 C -0.0883(4) 1.5995(4) 0.4566(2) 0.0841(11) Uani 1 1 d . . . H19 H -0.0514 1.6756 0.4783 0.101 Uiso 1 1 calc R . . C20 C -0.1848(3) 1.5314(3) 0.48252(16) 0.0661(9) Uani 1 1 d . . . H20 H -0.2121 1.5619 0.5217 0.079 Uiso 1 1 calc R . . C21 C -0.4475(3) 1.2975(2) 0.61706(12) 0.0453(6) Uani 1 1 d . . . H21 H -0.3701 1.3324 0.6390 0.054 Uiso 1 1 calc R . . C22 C -0.5446(3) 1.2283(2) 0.64935(12) 0.0442(6) Uani 1 1 d . . . C23 C -0.6696(3) 1.2004(3) 0.62410(14) 0.0672(9) Uani 1 1 d . . . H23 H -0.6949 1.2288 0.5870 0.081 Uiso 1 1 calc R . . C24 C -0.7559(3) 1.1307(4) 0.65408(16) 0.0785(11) Uani 1 1 d . . . H24 H -0.8391 1.1113 0.6357 0.094 Uiso 1 1 calc R . . C25 C -0.6089(3) 1.1204(2) 0.73385(12) 0.0490(6) Uani 1 1 d . . . H25 H -0.5874 1.0953 0.7724 0.059 Uiso 1 1 calc R . . C26 C -0.5154(3) 1.1883(2) 0.70631(12) 0.0454(6) Uani 1 1 d . . . H26 H -0.4330 1.2072 0.7259 0.055 Uiso 1 1 calc R . . N7 N 0.1952(2) 0.8012(2) 0.78706(11) 0.0543(6) Uani 1 1 d . . . N8 N 0.4093(2) 0.6840(2) 0.98112(10) 0.0475(5) Uani 1 1 d . . . N9 N 0.4270(2) 0.62288(19) 1.03372(10) 0.0424(5) Uani 1 1 d . . . N10 N 0.57663(19) 0.89592(19) 1.07448(10) 0.0423(5) Uani 1 1 d . . . N11 N 0.4634(2) 0.89558(19) 1.10608(10) 0.0441(5) Uani 1 1 d . . . N12 N 0.0422(2) 0.9991(2) 1.17924(10) 0.0526(6) Uani 1 1 d . . . C27 C 0.3497(3) 0.7872(3) 0.87093(17) 0.0745(10) Uani 1 1 d . . . H27 H 0.4285 0.8177 0.8926 0.089 Uiso 1 1 calc R . . C28 C 0.3076(4) 0.8385(3) 0.82054(19) 0.0813(12) Uani 1 1 d . . . H28 H 0.3604 0.9036 0.8087 0.098 Uiso 1 1 calc R . . C29 C 0.1256(2) 0.7027(2) 0.80326(12) 0.0464(6) Uani 1 1 d . . . H29 H 0.0490 0.6717 0.7796 0.056 Uiso 1 1 calc R . . C30 C 0.1614(2) 0.6449(2) 0.85302(12) 0.0425(5) Uani 1 1 d . . . H30 H 0.1099 0.5762 0.8621 0.051 Uiso 1 1 calc R . . C31 C 0.2742(2) 0.6895(2) 0.88939(12) 0.0423(5) Uani 1 1 d . . . C32 C 0.3111(2) 0.6361(2) 0.94547(12) 0.0435(6) Uani 1 1 d . . . H32 H 0.2618 0.5665 0.9550 0.052 Uiso 1 1 calc R . . C33 C 0.5236(2) 0.6749(2) 1.07125(11) 0.0367(5) Uani 1 1 d . . . C34 C 0.5533(2) 0.6219(2) 1.12945(11) 0.0396(5) Uani 1 1 d . . . C35 C 0.4580(3) 0.5476(3) 1.15345(13) 0.0578(7) Uani 1 1 d . . . H35 H 0.3761 0.5316 1.1332 0.069 Uiso 1 1 calc R . . C36 C 0.4848(4) 0.4975(3) 1.20743(15) 0.0737(10) Uani 1 1 d . . . H36 H 0.4204 0.4484 1.2235 0.088 Uiso 1 1 calc R . . C37 C 0.6053(4) 0.5191(3) 1.23786(15) 0.0734(10) Uani 1 1 d . . . H37 H 0.6228 0.4837 1.2739 0.088 Uiso 1 1 calc R . . C38 C 0.6995(3) 0.5932(3) 1.21463(14) 0.0626(8) Uani 1 1 d . . . H38 H 0.7812 0.6085 1.2351 0.075 Uiso 1 1 calc R . . C39 C 0.6742(3) 0.6455(3) 1.16103(12) 0.0493(6) Uani 1 1 d . . . H39 H 0.7384 0.6967 1.1460 0.059 Uiso 1 1 calc R . . C40 C 0.6069(2) 0.7882(2) 1.05895(10) 0.0355(5) Uani 1 1 d . . . C41 C 0.7288(2) 0.7741(2) 1.02998(11) 0.0369(5) Uani 1 1 d . . . C42 C 0.7416(3) 0.6675(2) 0.98970(12) 0.0468(6) Uani 1 1 d . . . H42 H 0.6721 0.6062 0.9794 0.056 Uiso 1 1 calc R . . C43 C 0.8576(3) 0.6521(3) 0.96483(15) 0.0618(8) Uani 1 1 d . . . H43 H 0.8657 0.5811 0.9373 0.074 Uiso 1 1 calc R . . C44 C 0.9608(3) 0.7418(3) 0.98090(15) 0.0649(8) Uani 1 1 d . . . H44 H 1.0392 0.7307 0.9649 0.078 Uiso 1 1 calc R . . C45 C 0.9484(3) 0.8478(3) 1.02063(14) 0.0594(8) Uani 1 1 d . . . H45 H 1.0185 0.9083 1.0312 0.071 Uiso 1 1 calc R . . C46 C 0.8333(2) 0.8649(3) 1.04474(13) 0.0498(6) Uani 1 1 d . . . H46 H 0.8253 0.9375 1.0710 0.060 Uiso 1 1 calc R . . C47 C 0.3878(2) 0.9647(2) 1.08777(12) 0.0422(5) Uani 1 1 d . . . H47 H 0.4077 1.0091 1.0549 0.051 Uiso 1 1 calc R . . C48 C 0.2676(2) 0.9748(2) 1.11870(11) 0.0401(5) Uani 1 1 d . . . C49 C 0.2084(3) 0.8806(3) 1.14748(13) 0.0501(6) Uani 1 1 d . . . H49 H 0.2435 0.8080 1.1474 0.060 Uiso 1 1 calc R . . C50 C 0.0972(3) 0.8961(3) 1.17619(13) 0.0555(7) Uani 1 1 d . . . H50 H 0.0576 0.8315 1.1946 0.067 Uiso 1 1 calc R . . C51 C 0.0998(3) 1.0880(3) 1.15078(13) 0.0517(6) Uani 1 1 d . . . H51 H 0.0634 1.1602 1.1520 0.062 Uiso 1 1 calc R . . C52 C 0.2097(3) 1.0798(2) 1.11970(12) 0.0457(6) Uani 1 1 d . . . H52 H 0.2446 1.1441 1.0996 0.055 Uiso 1 1 calc R . . B1 B 0.1266(3) 0.5896(3) 0.23480(18) 0.0583(8) Uani 1 1 d . . . F1 F 0.2219(3) 0.6758(3) 0.25555(19) 0.1475(13) Uani 1 1 d . . . F3 F 0.1230(4) 0.5749(4) 0.17144(15) 0.1699(15) Uani 1 1 d . . . F4 F 0.0136(2) 0.6280(3) 0.24804(17) 0.1322(11) Uani 1 1 d . . . F2 F 0.1341(3) 0.4833(3) 0.2539(2) 0.1697(17) 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 0.04857(14) 0.0983(2) 0.06434(15) 0.04677(14) 0.01035(10) 0.01967(12) N1 0.0504(13) 0.0632(15) 0.0539(13) 0.0191(12) -0.0026(11) 0.0110(12) N2 0.0676(16) 0.0448(13) 0.0621(14) 0.0120(11) -0.0224(12) 0.0066(12) N3 0.0704(16) 0.0425(13) 0.0568(14) 0.0074(10) -0.0218(12) 0.0096(11) N4 0.0547(13) 0.0427(12) 0.0408(11) 0.0078(9) 0.0087(9) -0.0035(10) N5 0.0554(13) 0.0505(13) 0.0436(12) 0.0098(10) 0.0108(10) -0.0042(11) N6 0.0553(14) 0.0710(16) 0.0502(13) 0.0205(12) 0.0056(11) -0.0056(12) C1 0.0589(17) 0.0489(16) 0.0583(16) 0.0059(13) -0.0071(13) 0.0140(13) C2 0.0607(18) 0.0607(19) 0.0549(16) 0.0031(14) -0.0102(14) 0.0078(15) C3 0.071(2) 0.0524(17) 0.0653(18) 0.0200(15) -0.0060(15) 0.0181(15) C4 0.075(2) 0.0464(16) 0.0651(18) 0.0104(14) -0.0161(15) 0.0107(15) C5 0.0520(15) 0.0451(15) 0.0533(15) 0.0133(12) -0.0065(12) 0.0078(12) C6 0.0611(18) 0.0432(15) 0.0596(17) 0.0079(13) -0.0155(14) 0.0067(13) C7 0.0518(15) 0.0376(13) 0.0409(12) 0.0065(10) -0.0008(11) 0.0079(11) C8 0.0560(15) 0.0399(13) 0.0392(12) 0.0086(10) -0.0010(11) 0.0072(12) C9 0.082(2) 0.0481(16) 0.0514(16) -0.0011(13) -0.0093(15) 0.0166(15) C10 0.090(2) 0.066(2) 0.0496(17) -0.0025(15) -0.0172(16) 0.0070(18) C11 0.069(2) 0.0636(19) 0.0560(17) 0.0224(15) -0.0148(14) 0.0049(16) C12 0.0641(18) 0.0465(16) 0.0675(18) 0.0214(14) -0.0093(15) 0.0098(14) C13 0.0622(17) 0.0367(13) 0.0494(14) 0.0094(11) -0.0032(12) 0.0062(12) C14 0.0491(14) 0.0365(13) 0.0377(12) 0.0086(10) 0.0028(10) 0.0073(11) C15 0.0523(15) 0.0487(15) 0.0391(12) 0.0125(11) 0.0066(11) 0.0063(12) C16 0.081(2) 0.091(3) 0.0474(16) -0.0042(16) 0.0173(16) -0.012(2) C17 0.100(3) 0.142(4) 0.055(2) 0.004(2) 0.035(2) -0.021(3) C18 0.082(3) 0.108(3) 0.080(2) 0.033(2) 0.029(2) -0.016(2) C19 0.084(3) 0.066(2) 0.097(3) 0.0097(19) 0.032(2) -0.0158(19) C20 0.077(2) 0.0533(18) 0.0659(19) 0.0045(14) 0.0282(16) -0.0043(16) C21 0.0483(14) 0.0429(14) 0.0433(13) 0.0061(11) 0.0078(11) -0.0008(11) C22 0.0514(15) 0.0395(13) 0.0406(13) 0.0062(10) 0.0091(11) 0.0001(11) C23 0.0579(18) 0.097(2) 0.0481(15) 0.0327(16) -0.0033(13) -0.0068(17) C24 0.0510(18) 0.121(3) 0.0608(19) 0.0398(19) -0.0057(14) -0.0218(19) C25 0.0557(16) 0.0494(15) 0.0435(13) 0.0138(11) 0.0058(12) 0.0051(12) C26 0.0460(14) 0.0454(14) 0.0446(13) 0.0080(11) 0.0033(11) 0.0039(11) N7 0.0542(14) 0.0531(14) 0.0563(13) 0.0153(11) -0.0099(11) 0.0076(11) N8 0.0487(12) 0.0448(12) 0.0474(12) 0.0144(9) -0.0085(10) -0.0027(10) N9 0.0429(11) 0.0409(11) 0.0433(11) 0.0136(9) -0.0019(9) -0.0004(9) N10 0.0399(11) 0.0385(11) 0.0485(11) 0.0054(9) 0.0078(9) 0.0051(9) N11 0.0431(11) 0.0425(12) 0.0489(12) 0.0066(9) 0.0106(9) 0.0111(9) N12 0.0519(13) 0.0649(15) 0.0460(12) 0.0157(11) 0.0123(10) 0.0155(11) C27 0.064(2) 0.0621(19) 0.093(2) 0.0398(18) -0.0358(18) -0.0222(16) C28 0.073(2) 0.068(2) 0.101(3) 0.050(2) -0.033(2) -0.0219(18) C29 0.0409(13) 0.0495(15) 0.0460(13) -0.0008(11) -0.0055(11) 0.0084(12) C30 0.0393(13) 0.0406(13) 0.0456(13) 0.0032(10) 0.0006(10) 0.0024(10) C31 0.0414(13) 0.0344(13) 0.0490(14) 0.0042(10) -0.0039(11) 0.0026(10) C32 0.0427(13) 0.0365(13) 0.0500(14) 0.0083(11) -0.0023(11) 0.0013(11) C33 0.0375(12) 0.0357(12) 0.0380(11) 0.0067(9) 0.0059(9) 0.0068(10) C34 0.0459(13) 0.0397(13) 0.0355(11) 0.0068(10) 0.0067(10) 0.0121(11) C35 0.0652(18) 0.0605(18) 0.0486(15) 0.0170(13) 0.0087(13) -0.0001(15) C36 0.100(3) 0.072(2) 0.0548(18) 0.0296(16) 0.0176(18) 0.006(2) C37 0.110(3) 0.076(2) 0.0462(16) 0.0234(15) 0.0126(18) 0.042(2) C38 0.068(2) 0.080(2) 0.0462(15) 0.0105(15) 0.0000(14) 0.0356(17) C39 0.0501(15) 0.0578(17) 0.0425(13) 0.0072(12) 0.0027(11) 0.0176(13) C40 0.0366(12) 0.0351(12) 0.0344(11) 0.0051(9) 0.0011(9) 0.0044(10) C41 0.0368(12) 0.0380(12) 0.0371(11) 0.0091(9) 0.0039(9) 0.0058(10) C42 0.0504(15) 0.0396(14) 0.0509(14) 0.0064(11) 0.0133(12) 0.0046(11) C43 0.068(2) 0.0587(18) 0.0633(18) 0.0053(14) 0.0225(15) 0.0207(16) C44 0.0456(16) 0.088(2) 0.0674(19) 0.0176(17) 0.0216(14) 0.0191(16) C45 0.0383(14) 0.076(2) 0.0604(17) 0.0091(15) 0.0048(12) -0.0026(14) C46 0.0409(14) 0.0534(16) 0.0508(15) 0.0002(12) 0.0034(11) -0.0007(12) C47 0.0419(13) 0.0398(13) 0.0458(13) 0.0086(10) 0.0051(10) 0.0054(11) C48 0.0407(13) 0.0428(13) 0.0370(12) 0.0062(10) 0.0011(10) 0.0068(10) C49 0.0531(16) 0.0470(15) 0.0543(15) 0.0132(12) 0.0099(12) 0.0139(12) C50 0.0591(17) 0.0569(17) 0.0551(16) 0.0179(13) 0.0164(13) 0.0097(14) C51 0.0543(16) 0.0597(17) 0.0470(14) 0.0138(12) 0.0078(12) 0.0224(13) C52 0.0482(14) 0.0485(15) 0.0444(13) 0.0147(11) 0.0074(11) 0.0121(12) B1 0.0447(17) 0.060(2) 0.070(2) 0.0181(17) 0.0019(15) -0.0022(16) F1 0.0835(18) 0.113(2) 0.225(4) 0.015(2) -0.044(2) -0.0305(16) F3 0.217(4) 0.189(4) 0.091(2) -0.006(2) 0.021(2) 0.005(3) F4 0.0698(15) 0.158(3) 0.186(3) 0.063(2) 0.0288(17) 0.0319(16) F2 0.104(2) 0.112(2) 0.315(5) 0.124(3) -0.014(3) 0.0081(17) _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 N7 2.285(2) . ? Ag1 N1 2.336(2) . ? Ag1 N6 2.366(2) 1_655 ? Ag1 N12 2.441(2) 2_577 ? N1 C3 1.320(4) . ? N1 C2 1.338(4) . ? N2 C6 1.266(4) . ? N2 N3 1.409(3) . ? N3 C7 1.278(3) . ? N4 C14 1.279(3) . ? N4 N5 1.402(3) . ? N5 C21 1.267(3) . ? N6 C25 1.327(4) . ? N6 C24 1.341(4) . ? N6 Ag1 2.366(2) 1_455 ? C1 C2 1.369(4) . ? C1 C5 1.379(4) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 C4 1.380(4) . ? C3 H3 0.9300 . ? C4 C5 1.382(4) . ? C4 H4 0.9300 . ? C5 C6 1.458(4) . ? C6 H6 0.9300 . ? C7 C8 1.474(4) . ? C7 C14 1.505(3) . ? C8 C13 1.380(4) . ? C8 C9 1.393(4) . ? C9 C10 1.378(4) . ? C9 H9 0.9300 . ? C10 C11 1.376(5) . ? C10 H10 0.9300 . ? C11 C12 1.364(4) . ? C11 H11 0.9300 . ? C12 C13 1.383(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.477(4) . ? C15 C16 1.380(4) . ? C15 C20 1.389(4) . ? C16 C17 1.377(5) . ? C16 H16 0.9300 . ? C17 C18 1.362(6) . ? C17 H17 0.9300 . ? C18 C19 1.361(5) . ? C18 H18 0.9300 . ? C19 C20 1.379(4) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.464(3) . ? C21 H21 0.9300 . ? C22 C23 1.379(4) . ? C22 C26 1.383(4) . ? C23 C24 1.366(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.375(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? N7 C29 1.337(4) . ? N7 C28 1.338(4) . ? N8 C32 1.263(3) . ? N8 N9 1.406(3) . ? N9 C33 1.283(3) . ? N10 C40 1.280(3) . ? N10 N11 1.406(3) . ? N11 C47 1.260(3) . ? N12 C51 1.331(4) . ? N12 C50 1.341(4) . ? N12 Ag1 2.441(2) 2_577 ? C27 C28 1.364(4) . ? C27 C31 1.380(4) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.375(4) . ? C29 H29 0.9300 . ? C30 C31 1.381(3) . ? C30 H30 0.9300 . ? C31 C32 1.462(4) . ? C32 H32 0.9300 . ? C33 C34 1.481(3) . ? C33 C40 1.505(3) . ? C34 C35 1.387(4) . ? C34 C39 1.388(4) . ? C35 C36 1.378(4) . ? C35 H35 0.9300 . ? C36 C37 1.374(5) . ? C36 H36 0.9300 . ? C37 C38 1.370(5) . ? C37 H37 0.9300 . ? C38 C39 1.381(4) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.476(3) . ? C41 C42 1.386(3) . ? C41 C46 1.388(4) . ? C42 C43 1.383(4) . ? C42 H42 0.9300 . ? C43 C44 1.373(5) . ? C43 H43 0.9300 . ? C44 C45 1.374(5) . ? C44 H44 0.9300 . ? C45 C46 1.371(4) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.473(3) . ? C47 H47 0.9300 . ? C48 C52 1.382(4) . ? C48 C49 1.386(4) . ? C49 C50 1.374(4) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.375(4) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? B1 F1 1.309(4) . ? B1 F2 1.313(4) . ? B1 F3 1.334(5) . ? B1 F4 1.350(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Ag1 N1 136.55(9) . . ? N7 Ag1 N6 110.83(9) . 1_655 ? N1 Ag1 N6 96.25(9) . 1_655 ? N7 Ag1 N12 98.83(9) . 2_577 ? N1 Ag1 N12 90.70(8) . 2_577 ? N6 Ag1 N12 126.52(9) 1_655 2_577 ? C3 N1 C2 117.0(2) . . ? C3 N1 Ag1 127.6(2) . . ? C2 N1 Ag1 115.34(19) . . ? C6 N2 N3 112.2(2) . . ? C7 N3 N2 113.0(2) . . ? C14 N4 N5 115.0(2) . . ? C21 N5 N4 112.6(2) . . ? C25 N6 C24 116.1(2) . . ? C25 N6 Ag1 127.54(19) . 1_455 ? C24 N6 Ag1 116.1(2) . 1_455 ? C2 C1 C5 119.0(3) . . ? C2 C1 H1 120.5 . . ? C5 C1 H1 120.5 . . ? N1 C2 C1 123.7(3) . . ? N1 C2 H2 118.2 . . ? C1 C2 H2 118.2 . . ? N1 C3 C4 123.2(3) . . ? N1 C3 H3 118.4 . . ? C4 C3 H3 118.4 . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C1 C5 C4 117.6(3) . . ? C1 C5 C6 121.5(3) . . ? C4 C5 C6 120.9(3) . . ? N2 C6 C5 119.7(3) . . ? N2 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? N3 C7 C8 117.9(2) . . ? N3 C7 C14 123.2(2) . . ? C8 C7 C14 118.9(2) . . ? C13 C8 C9 119.0(3) . . ? C13 C8 C7 120.8(2) . . ? C9 C8 C7 120.2(2) . . ? C10 C9 C8 119.8(3) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.5(3) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.0(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.2(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C13 C12 120.5(3) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? N4 C14 C15 118.2(2) . . ? N4 C14 C7 123.4(2) . . ? C15 C14 C7 118.4(2) . . ? C16 C15 C20 117.9(3) . . ? C16 C15 C14 121.5(3) . . ? C20 C15 C14 120.6(2) . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 121.1(3) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C17 119.3(3) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 120.8(3) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? N5 C21 C22 120.2(2) . . ? N5 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C26 117.1(2) . . ? C23 C22 C21 121.2(2) . . ? C26 C22 C21 121.7(2) . . ? C24 C23 C22 119.4(3) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? N6 C24 C23 124.1(3) . . ? N6 C24 H24 118.0 . . ? C23 C24 H24 118.0 . . ? N6 C25 C26 123.7(3) . . ? N6 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C25 C26 C22 119.6(3) . . ? C25 C26 H26 120.2 . . ? C22 C26 H26 120.2 . . ? C29 N7 C28 115.9(2) . . ? C29 N7 Ag1 123.84(18) . . ? C28 N7 Ag1 114.9(2) . . ? C32 N8 N9 112.4(2) . . ? C33 N9 N8 112.2(2) . . ? C40 N10 N11 113.0(2) . . ? C47 N11 N10 114.6(2) . . ? C51 N12 C50 116.2(2) . . ? C51 N12 Ag1 119.08(18) . 2_577 ? C50 N12 Ag1 122.05(18) . 2_577 ? C28 C27 C31 119.4(3) . . ? C28 C27 H27 120.3 . . ? C31 C27 H27 120.3 . . ? N7 C28 C27 124.3(3) . . ? N7 C28 H28 117.9 . . ? C27 C28 H28 117.9 . . ? N7 C29 C30 123.5(2) . . ? N7 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? C29 C30 C31 119.6(2) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C27 C31 C30 117.2(2) . . ? C27 C31 C32 121.6(2) . . ? C30 C31 C32 121.3(2) . . ? N8 C32 C31 120.5(2) . . ? N8 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? N9 C33 C34 118.5(2) . . ? N9 C33 C40 122.7(2) . . ? C34 C33 C40 118.8(2) . . ? C35 C34 C39 119.0(2) . . ? C35 C34 C33 119.4(2) . . ? C39 C34 C33 121.6(2) . . ? C36 C35 C34 119.8(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 121.1(3) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C38 C37 C36 119.3(3) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 120.5(3) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C34 120.3(3) . . ? C38 C39 H39 119.9 . . ? C34 C39 H39 119.9 . . ? N10 C40 C41 119.4(2) . . ? N10 C40 C33 121.9(2) . . ? C41 C40 C33 118.6(2) . . ? C42 C41 C46 119.2(2) . . ? C42 C41 C40 120.2(2) . . ? C46 C41 C40 120.5(2) . . ? C43 C42 C41 120.1(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 119.9(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.2(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 120.4(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 120.1(3) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? N11 C47 C48 119.6(2) . . ? N11 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C52 C48 C49 117.7(2) . . ? C52 C48 C47 120.5(2) . . ? C49 C48 C47 121.8(2) . . ? C50 C49 C48 119.1(3) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? N12 C50 C49 123.8(3) . . ? N12 C50 H50 118.1 . . ? C49 C50 H50 118.1 . . ? N12 C51 C52 124.1(3) . . ? N12 C51 H51 117.9 . . ? C52 C51 H51 117.9 . . ? C51 C52 C48 119.0(3) . . ? C51 C52 H52 120.5 . . ? C48 C52 H52 120.5 . . ? F1 B1 F2 115.3(3) . . ? F1 B1 F3 106.5(4) . . ? F2 B1 F3 109.1(4) . . ? F1 B1 F4 111.0(4) . . ? F2 B1 F4 110.4(3) . . ? F3 B1 F4 103.7(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.934 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.056 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 748792' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H26 Ag N7 O4' _chemical_formula_weight 632.43 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 'Cc ' _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' _cell_length_a 12.162(9) _cell_length_b 13.554(9) _cell_length_c 17.423(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.672(19) _cell_angle_gamma 90.00 _cell_volume 2853(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2249 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.77 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.752 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7763 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3681 _reflns_number_gt 2491 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The NO~3~^-^ anion is rotationally disordered over two orientations in the refined ratio 0.5:0.5. To assist the refinement, all N-O bonds were restrained to be similar. 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^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.24(4) _refine_ls_number_reflns 3681 _refine_ls_number_parameters 398 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.976 _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 0.56272(7) 0.07166(5) 0.22891(5) 0.1250(3) Uani 1 1 d . . . N1 N 0.6950(5) -0.0347(4) 0.2591(4) 0.0825(15) Uani 1 1 d . . . N6 N 1.3973(6) -0.1193(4) 0.6869(3) 0.0888(17) Uani 1 1 d . . . C21 C 1.0768(5) -0.2437(4) 0.6318(4) 0.0735(16) Uani 1 1 d . . . H21A H 1.0199 -0.2269 0.6606 0.088 Uiso 1 1 calc R . . N5 N 1.0608(4) -0.3044(4) 0.5772(3) 0.0709(12) Uani 1 1 d . . . N2 N 0.9342(4) -0.3057(3) 0.3790(3) 0.0650(12) Uani 1 1 d . . . N3 N 1.0262(4) -0.3693(3) 0.3937(3) 0.0609(11) Uani 1 1 d . . . C2 C 0.6741(6) -0.1132(5) 0.3004(4) 0.0802(17) Uani 1 1 d . . . H2A H 0.6022 -0.1236 0.3118 0.096 Uiso 1 1 calc R A . C1 C 0.7551(5) -0.1798(4) 0.3270(4) 0.0744(17) Uani 1 1 d . . . H1A H 0.7382 -0.2335 0.3567 0.089 Uiso 1 1 calc R . . C5 C 0.8621(5) -0.1660(4) 0.3090(3) 0.0620(14) Uani 1 1 d . . . C4 C 0.8844(6) -0.0848(4) 0.2653(4) 0.0773(18) Uani 1 1 d . . . H4A H 0.9553 -0.0730 0.2523 0.093 Uiso 1 1 calc R . . C3 C 0.7960(8) -0.0206(5) 0.2409(5) 0.095(2) Uani 1 1 d . . . H3A H 0.8094 0.0339 0.2109 0.114 Uiso 1 1 calc R A . C6 C 0.9516(5) -0.2360(4) 0.3347(3) 0.0602(13) Uani 1 1 d . . . H6A H 1.0210 -0.2284 0.3180 0.072 Uiso 1 1 calc R . . C7 C 1.0256(5) -0.4158(3) 0.4573(4) 0.0540(14) Uani 1 1 d . . . C8 C 1.1200(5) -0.4822(4) 0.4830(3) 0.0609(14) Uani 1 1 d . . . C9 C 1.2242(5) -0.4628(5) 0.4586(5) 0.0845(19) Uani 1 1 d . . . H9A H 1.2355 -0.4096 0.4267 0.101 Uiso 1 1 calc R . . C10 C 1.3090(6) -0.5271(8) 0.4847(6) 0.105(3) Uani 1 1 d . . . H10A H 1.3792 -0.5153 0.4705 0.126 Uiso 1 1 calc R . . C11 C 1.2945(8) -0.6068(7) 0.5303(6) 0.112(3) Uani 1 1 d . . . H11A H 1.3532 -0.6493 0.5453 0.135 Uiso 1 1 calc R . . C12 C 1.1948(9) -0.6233(6) 0.5533(5) 0.103(3) Uani 1 1 d . . . H12A H 1.1849 -0.6766 0.5854 0.123 Uiso 1 1 calc R . . C13 C 1.1055(7) -0.5613(5) 0.5296(5) 0.081(2) Uani 1 1 d . . . H13A H 1.0364 -0.5737 0.5455 0.097 Uiso 1 1 calc R . . C14 C 0.9362(4) -0.4010(4) 0.5098(3) 0.0546(12) Uani 1 1 d . . . C15 C 0.8311(4) -0.4554(4) 0.4941(4) 0.0576(13) Uani 1 1 d . . . C16 C 0.8130(5) -0.5212(5) 0.4334(4) 0.0734(16) Uani 1 1 d . . . H16A H 0.8672 -0.5303 0.4006 0.088 Uiso 1 1 calc R . . C17 C 0.7148(6) -0.5736(5) 0.4210(5) 0.095(2) Uani 1 1 d . . . H17A H 0.7034 -0.6179 0.3801 0.114 Uiso 1 1 calc R . . C18 C 0.6339(5) -0.5602(6) 0.4693(5) 0.089(2) Uani 1 1 d . . . H18A H 0.5687 -0.5966 0.4618 0.107 Uiso 1 1 calc R . . C19 C 0.6494(5) -0.4938(6) 0.5279(5) 0.0855(19) Uani 1 1 d . . . H19A H 0.5940 -0.4836 0.5595 0.103 Uiso 1 1 calc R . . C20 C 0.7469(5) -0.4417(4) 0.5406(4) 0.0677(15) Uani 1 1 d . . . H20A H 0.7565 -0.3965 0.5810 0.081 Uiso 1 1 calc R . . N4 N 0.9525(4) -0.3458(4) 0.5694(3) 0.0699(12) Uani 1 1 d . . . C22 C 1.1873(6) -0.1998(4) 0.6493(3) 0.0691(16) Uani 1 1 d . . . C23 C 1.2035(6) -0.1221(5) 0.7007(4) 0.0837(19) Uani 1 1 d . . . H23A H 1.1447 -0.0961 0.7238 0.100 Uiso 1 1 calc R . . C24 C 1.3080(8) -0.0840(4) 0.7169(4) 0.088(2) Uani 1 1 d . . . H24A H 1.3178 -0.0307 0.7506 0.106 Uiso 1 1 calc R . . C25 C 1.3798(6) -0.1952(5) 0.6370(4) 0.0848(19) Uani 1 1 d . . . H25A H 1.4402 -0.2210 0.6156 0.102 Uiso 1 1 calc R . . C26 C 1.2783(6) -0.2360(4) 0.6163(4) 0.0756(17) Uani 1 1 d . . . H26A H 1.2699 -0.2874 0.5808 0.091 Uiso 1 1 calc R . . N7 N 0.7235(12) 0.2900(10) 0.2315(9) 0.071(5) Uani 0.50 1 d PD A 1 O1 O 0.8054(15) 0.3436(14) 0.2475(14) 0.133(6) Uani 0.50 1 d PD A 1 O2 O 0.7210(15) 0.2097(14) 0.2651(12) 0.119(7) Uani 0.50 1 d PD A 1 O3 O 0.6368(15) 0.3270(15) 0.2000(15) 0.124(7) Uani 0.50 1 d PD A 1 N7' N 0.6739(18) 0.2890(13) 0.2209(18) 0.135(12) Uani 0.50 1 d PD B 2 O1' O 0.721(3) 0.3643(15) 0.2400(16) 0.231(19) Uani 0.50 1 d PD B 2 O2' O 0.722(2) 0.2122(19) 0.2306(14) 0.180(14) Uani 0.50 1 d PD B 2 O3' O 0.5933(19) 0.292(2) 0.175(2) 0.192(14) Uani 0.50 1 d PD B 2 O4 O 0.9786(9) 0.2049(10) 0.2965(7) 0.217(5) Uani 1 1 d . . . H4B H 0.9239 0.2441 0.2895 0.260 Uiso 1 1 d R . . C27 C 0.9824(12) 0.1592(10) 0.3644(9) 0.160(4) Uani 1 1 d . . . H27B H 1.0541 0.1276 0.3750 0.192 Uiso 1 1 calc R . . H27A H 0.9269 0.1074 0.3599 0.192 Uiso 1 1 calc R . . C28 C 0.9654(15) 0.2183(9) 0.4283(10) 0.195(6) Uani 1 1 d . . . H28A H 0.9725 0.1786 0.4742 0.292 Uiso 1 1 calc R . . H28B H 0.8926 0.2466 0.4205 0.292 Uiso 1 1 calc R . . H28C H 1.0196 0.2701 0.4338 0.292 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 Ag1 0.1262(5) 0.1037(4) 0.1437(6) 0.0269(4) 0.0092(4) 0.0623(4) N1 0.092(4) 0.058(3) 0.096(4) 0.006(3) 0.005(3) 0.019(3) N6 0.108(5) 0.078(3) 0.078(4) -0.011(3) -0.001(3) -0.042(3) C21 0.069(4) 0.069(3) 0.079(4) -0.008(3) -0.009(3) 0.013(3) N5 0.074(3) 0.069(3) 0.071(3) -0.016(3) 0.010(2) -0.011(2) N2 0.054(3) 0.070(3) 0.072(3) 0.015(3) 0.010(2) 0.014(2) N3 0.057(3) 0.064(3) 0.063(3) 0.007(2) 0.011(2) 0.010(2) C2 0.075(4) 0.070(4) 0.093(5) 0.005(4) -0.001(3) 0.014(3) C1 0.081(4) 0.053(3) 0.088(5) 0.003(3) 0.005(3) 0.009(3) C5 0.064(3) 0.050(3) 0.069(4) 0.000(3) -0.002(3) 0.002(2) C4 0.079(4) 0.059(3) 0.096(5) 0.013(3) 0.015(4) 0.002(3) C3 0.124(7) 0.067(4) 0.093(5) 0.021(4) 0.009(5) 0.021(4) C6 0.064(3) 0.051(3) 0.067(4) 0.000(3) 0.016(3) 0.003(2) C7 0.046(3) 0.046(3) 0.070(4) 0.002(3) 0.004(3) 0.004(2) C8 0.062(3) 0.063(3) 0.056(3) -0.010(3) 0.000(3) 0.011(3) C9 0.058(4) 0.087(4) 0.107(6) -0.002(4) 0.003(3) 0.007(3) C10 0.063(4) 0.137(7) 0.113(6) -0.002(6) -0.003(4) 0.038(5) C11 0.082(6) 0.111(6) 0.132(8) -0.027(6) -0.039(5) 0.051(5) C12 0.129(8) 0.076(5) 0.096(6) 0.012(4) -0.018(5) 0.030(5) C13 0.079(4) 0.086(5) 0.078(5) 0.013(4) 0.009(4) 0.015(3) C14 0.055(3) 0.051(3) 0.056(3) 0.004(3) 0.004(2) 0.007(2) C15 0.045(3) 0.062(3) 0.063(4) 0.005(3) -0.002(3) 0.009(2) C16 0.065(4) 0.087(4) 0.068(4) -0.008(3) 0.007(3) -0.005(3) C17 0.065(4) 0.112(6) 0.106(6) -0.024(4) -0.002(4) -0.009(4) C18 0.056(4) 0.114(5) 0.096(6) 0.002(4) -0.003(4) -0.010(3) C19 0.050(4) 0.111(5) 0.096(5) 0.007(5) 0.014(3) 0.008(3) C20 0.061(4) 0.080(4) 0.062(4) -0.004(3) 0.010(3) 0.010(3) N4 0.066(3) 0.075(3) 0.068(3) -0.006(3) 0.006(2) 0.003(2) C22 0.092(4) 0.060(3) 0.050(3) 0.005(3) -0.014(3) -0.007(3) C23 0.097(5) 0.068(4) 0.080(4) -0.022(3) -0.016(4) 0.012(3) C24 0.132(7) 0.053(3) 0.078(5) -0.012(3) 0.001(5) -0.003(4) C25 0.100(5) 0.083(4) 0.073(4) -0.016(4) 0.019(4) -0.034(4) C26 0.086(5) 0.067(3) 0.073(4) -0.011(3) 0.005(3) -0.013(3) N7 0.097(15) 0.063(10) 0.061(7) -0.006(7) 0.040(8) 0.015(8) O1 0.167(15) 0.081(10) 0.167(14) -0.009(8) 0.080(13) -0.016(11) O2 0.155(12) 0.088(11) 0.112(18) 0.045(11) 0.009(10) -0.026(8) O3 0.109(17) 0.109(16) 0.158(19) 0.064(15) 0.030(12) 0.010(11) N7' 0.11(2) 0.11(2) 0.20(3) 0.058(19) 0.09(2) 0.034(19) O1' 0.43(6) 0.076(13) 0.21(3) -0.032(12) 0.14(4) -0.09(2) O2' 0.33(3) 0.103(16) 0.104(19) -0.015(13) 0.026(17) 0.006(16) O3' 0.103(16) 0.25(3) 0.24(3) -0.02(2) 0.058(16) -0.025(15) O4 0.157(8) 0.306(13) 0.190(10) 0.072(10) 0.033(7) -0.044(8) C27 0.190(13) 0.156(10) 0.140(10) 0.010(9) 0.042(9) -0.015(9) C28 0.268(18) 0.131(10) 0.181(14) -0.048(9) 0.012(12) -0.028(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N6 2.158(6) 2_454 ? Ag1 N1 2.179(5) . ? Ag1 O2 2.706(17) . ? N1 C3 1.318(10) . ? N1 C2 1.324(9) . ? N6 C24 1.346(10) . ? N6 C25 1.347(8) . ? N6 Ag1 2.158(6) 2_655 ? C21 N5 1.255(8) . ? C21 C22 1.469(9) . ? C21 H21A 0.9300 . ? N5 N4 1.424(7) . ? N2 C6 1.254(7) . ? N2 N3 1.411(6) . ? N3 C7 1.276(7) . ? C2 C1 1.377(8) . ? C2 H2A 0.9300 . ? C1 C5 1.387(8) . ? C1 H1A 0.9300 . ? C5 C4 1.383(8) . ? C5 C6 1.473(7) . ? C4 C3 1.410(10) . ? C4 H4A 0.9300 . ? C3 H3A 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.487(8) . ? C7 C14 1.513(8) . ? C8 C13 1.368(9) . ? C8 C9 1.407(9) . ? C9 C10 1.387(10) . ? C9 H9A 0.9300 . ? C10 C11 1.365(15) . ? C10 H10A 0.9300 . ? C11 C12 1.340(12) . ? C11 H11A 0.9300 . ? C12 C13 1.397(11) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 N4 1.276(7) . ? C14 C15 1.474(8) . ? C15 C16 1.380(9) . ? C15 C20 1.391(8) . ? C16 C17 1.385(10) . ? C16 H16A 0.9300 . ? C17 C18 1.379(11) . ? C17 H17A 0.9300 . ? C18 C19 1.357(11) . ? C18 H18A 0.9300 . ? C19 C20 1.375(9) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C22 C26 1.393(9) . ? C22 C23 1.382(9) . ? C23 C24 1.370(11) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.362(9) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? N7 O3 1.236(14) . ? N7 O2 1.237(15) . ? N7 O1 1.239(14) . ? N7' O3' 1.195(19) . ? N7' O2' 1.197(19) . ? N7' O1' 1.197(19) . ? O4 C27 1.332(15) . ? O4 H4B 0.8500 . ? C27 C28 1.407(18) . ? C27 H27B 0.9700 . ? C27 H27A 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 N6 Ag1 N1 155.9(2) 2_454 . ? N6 Ag1 O2 118.8(5) 2_454 . ? N1 Ag1 O2 85.2(5) . . ? C3 N1 C2 119.4(6) . . ? C3 N1 Ag1 121.9(5) . . ? C2 N1 Ag1 118.7(5) . . ? C24 N6 C25 116.6(6) . . ? C24 N6 Ag1 121.6(5) . 2_655 ? C25 N6 Ag1 121.2(6) . 2_655 ? N5 C21 C22 118.7(6) . . ? N5 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? C21 N5 N4 113.1(5) . . ? C6 N2 N3 112.7(4) . . ? C7 N3 N2 112.0(4) . . ? N1 C2 C1 122.3(6) . . ? N1 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? C5 C1 C2 119.3(6) . . ? C5 C1 H1A 120.4 . . ? C2 C1 H1A 120.4 . . ? C1 C5 C4 118.8(5) . . ? C1 C5 C6 121.6(5) . . ? C4 C5 C6 119.6(5) . . ? C5 C4 C3 117.7(7) . . ? C5 C4 H4A 121.1 . . ? C3 C4 H4A 121.1 . . ? N1 C3 C4 122.5(7) . . ? N1 C3 H3A 118.8 . . ? C4 C3 H3A 118.8 . . ? N2 C6 C5 120.1(5) . . ? N2 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? N3 C7 C8 118.6(5) . . ? N3 C7 C14 122.4(5) . . ? C8 C7 C14 118.8(5) . . ? C13 C8 C9 120.6(6) . . ? C13 C8 C7 120.3(6) . . ? C9 C8 C7 119.1(5) . . ? C10 C9 C8 116.4(7) . . ? C10 C9 H9A 121.8 . . ? C8 C9 H9A 121.8 . . ? C11 C10 C9 123.2(8) . . ? C11 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? C12 C11 C10 119.3(7) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 120.7(8) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C8 C13 C12 119.8(8) . . ? C8 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? N4 C14 C15 119.6(5) . . ? N4 C14 C7 121.1(5) . . ? C15 C14 C7 119.3(5) . . ? C16 C15 C20 118.0(5) . . ? C16 C15 C14 121.5(5) . . ? C20 C15 C14 120.4(5) . . ? C17 C16 C15 120.6(6) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C18 C17 C16 120.1(7) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? C19 C18 C17 119.9(6) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 120.3(6) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C15 121.1(6) . . ? C19 C20 H20A 119.5 . . ? C15 C20 H20A 119.5 . . ? C14 N4 N5 111.3(5) . . ? C26 C22 C23 118.4(6) . . ? C26 C22 C21 121.6(5) . . ? C23 C22 C21 120.0(6) . . ? C24 C23 C22 118.6(7) . . ? C24 C23 H23A 120.7 . . ? C22 C23 H23A 120.7 . . ? N6 C24 C23 123.9(6) . . ? N6 C24 H24A 118.1 . . ? C23 C24 H24A 118.1 . . ? N6 C25 C26 123.4(7) . . ? N6 C25 H25A 118.3 . . ? C26 C25 H25A 118.3 . . ? C25 C26 C22 119.1(6) . . ? C25 C26 H26A 120.5 . . ? C22 C26 H26A 120.5 . . ? O3 N7 O2 120.0(11) . . ? O3 N7 O1 118.9(11) . . ? O2 N7 O1 118.2(11) . . ? N7 O2 Ag1 123.6(11) . . ? O3' N7' O2' 118.5(13) . . ? O3' N7' O1' 118.8(13) . . ? O2' N7' O1' 119.6(13) . . ? C27 O4 H4B 111.3 . . ? O4 C27 C28 116.4(14) . . ? O4 C27 H27B 108.2 . . ? C28 C27 H27B 108.2 . . ? O4 C27 H27A 108.2 . . ? C28 C27 H27A 108.2 . . ? H27B C27 H27A 107.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.445 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.044 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 748793' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H43 N15 S2 Zn' _chemical_formula_weight 1055.54 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.062(7) _cell_length_b 9.816(3) _cell_length_c 23.111(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.780(6) _cell_angle_gamma 90.00 _cell_volume 5443(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1034 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 24.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0179 _exptl_absorpt_correction_T_max 0.0464 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27068 _diffrn_reflns_av_R_equivalents 0.1780 _diffrn_reflns_av_sigmaI/netI 0.2886 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9569 _reflns_number_gt 2212 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Since the quality of the single crystal was not stisfactory,the observed/unique reflection ratio was only 23%. 83 restraints and the third parameter of WGHT were applied to assist the refinement. The CH~3~CN is rotationally disordered over two orientations in the refined ratio 0.5:0.5. It was refined with distance restraints and the thermal parameters were also restrained to be similar. C-C bonds were restrained to 1.48 \%A. C-N bonds were restrained to 1.20 \%A. The distance of the two terminal atoms of CH~3~CN molecule was restrained to 2.7 \%A. C(8)-C(13), C(42), C(43) and C(45) of ligand were refined with restraints for the anisotropic displacement parameters. The thermal parameters on adjacent atoms C(53), S(1) and C(54), S(2) were restrained to be similar. 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 [0.00000+1.00000exp(5.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0111P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 9569 _refine_ls_number_parameters 666 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.2630 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.067 _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 Zn1 Zn -1.30328(3) 1.11889(7) -0.68560(3) 0.0745(2) Uani 1 1 d . . . C1 C -1.1964(2) 0.8680(6) -0.7686(3) 0.105(2) Uani 1 1 d . . . H1A H -1.1939 0.7750 -0.7749 0.126 Uiso 1 1 calc R . . N1 N -1.23982(19) 1.0494(4) -0.7291(2) 0.0770(16) Uani 1 1 d . . . C2 C -1.2328(3) 0.9151(6) -0.7385(3) 0.094(2) Uani 1 1 d . . . H2A H -1.2534 0.8520 -0.7239 0.113 Uiso 1 1 calc R . . N2 N -1.1140(2) 0.7831(5) -0.8220(2) 0.0932(18) Uani 1 1 d . . . C3 C -1.2071(3) 1.1319(6) -0.7494(3) 0.101(2) Uani 1 1 d . . . H3A H -1.2092 1.2245 -0.7419 0.121 Uiso 1 1 calc R . . N3 N -1.0721(2) 0.7561(5) -0.8501(2) 0.0886(17) Uani 1 1 d . . . C4 C -1.1706(3) 1.0921(6) -0.7801(3) 0.103(2) Uani 1 1 d . . . H4A H -1.1504 1.1564 -0.7947 0.123 Uiso 1 1 calc R . . N4 N -1.1064(2) 0.4471(4) -0.8177(2) 0.0795(17) Uani 1 1 d . . . C5 C -1.1644(3) 0.9549(6) -0.7892(3) 0.079(2) Uani 1 1 d . . . N5 N -1.1262(2) 0.4348(5) -0.8796(2) 0.0849(18) Uani 1 1 d . . . C6 C -1.1242(3) 0.9073(6) -0.8184(3) 0.082(2) Uani 1 1 d . . . H6A H -1.1054 0.9707 -0.8351 0.099 Uiso 1 1 calc R . . N6 N -1.25028(19) 0.4394(4) -1.0948(2) 0.0741(15) Uani 1 1 d . . . N7 N -1.36719(19) 1.1820(4) -0.6408(2) 0.0693(15) Uani 1 1 d . . . N8 N -1.5410(2) 1.3175(4) -0.5898(2) 0.0746(16) Uani 1 1 d . . . N9 N -1.57883(19) 1.3847(5) -0.5655(2) 0.0737(15) Uani 1 1 d . . . C7 C -1.0510(2) 0.6367(6) -0.8369(3) 0.0790(19) Uani 1 1 d . . . C8 C -1.0059(3) 0.5921(6) -0.8616(3) 0.086(2) Uani 1 1 d U . . C9 C -0.9765(3) 0.4726(6) -0.8427(3) 0.102(2) Uani 1 1 d U . . H9A H -0.9860 0.4179 -0.8144 0.122 Uiso 1 1 calc R . . C10 C -0.9323(3) 0.4324(7) -0.8656(3) 0.120(3) Uani 1 1 d U . . H10A H -0.9111 0.3559 -0.8501 0.144 Uiso 1 1 calc R . . C11 C -0.9215(3) 0.5036(8) -0.9087(4) 0.145(3) Uani 1 1 d U . . H11A H -0.8937 0.4745 -0.9251 0.175 Uiso 1 1 calc R . . C12 C -0.9500(4) 0.6183(9) -0.9297(4) 0.170(3) Uani 1 1 d U . . H12A H -0.9416 0.6675 -0.9603 0.204 Uiso 1 1 calc R . . C13 C -0.9928(3) 0.6646(8) -0.9055(4) 0.145(3) Uani 1 1 d U . . H13A H -1.0118 0.7447 -0.9198 0.173 Uiso 1 1 calc R . . N10 N -1.5602(2) 1.0963(4) -0.4934(2) 0.0756(16) Uani 1 1 d . . . N11 N -1.5231(2) 1.1840(5) -0.4543(2) 0.0778(17) Uani 1 1 d . . . N12 N -1.36152(18) 1.2974(4) -0.2692(2) 0.0645(14) Uani 1 1 d . . . C14 C -1.0701(2) 0.5395(6) -0.7961(3) 0.074(2) Uani 1 1 d . . . C15 C -1.0463(3) 0.5545(6) -0.7302(3) 0.075(2) Uani 1 1 d . . . C16 C -1.0729(3) 0.4940(7) -0.6917(3) 0.113(3) Uani 1 1 d . . . H16A H -1.1054 0.4439 -0.7073 0.136 Uiso 1 1 calc R . . C17 C -1.0506(4) 0.5091(8) -0.6307(3) 0.133(3) Uani 1 1 d . . . H17A H -1.0685 0.4657 -0.6057 0.159 Uiso 1 1 calc R . . C18 C -1.0038(4) 0.5837(8) -0.6036(4) 0.143(4) Uani 1 1 d . . . H18A H -0.9902 0.5916 -0.5618 0.172 Uiso 1 1 calc R . . C19 C -0.9775(3) 0.6479(7) -0.6428(3) 0.122(3) Uani 1 1 d . . . H19A H -0.9454 0.6993 -0.6268 0.146 Uiso 1 1 calc R . . C20 C -0.9991(3) 0.6348(6) -0.7044(3) 0.097(2) Uani 1 1 d . . . H20A H -0.9820 0.6802 -0.7296 0.117 Uiso 1 1 calc R . . C21 C -1.1694(3) 0.4990(6) -0.9072(3) 0.079(2) Uani 1 1 d . . . H21A H -1.1848 0.5592 -0.8854 0.095 Uiso 1 1 calc R . . C22 C -1.1962(3) 0.4835(6) -0.9710(3) 0.079(2) Uani 1 1 d . . . C23 C -1.2407(3) 0.5579(6) -1.0019(3) 0.090(2) Uani 1 1 d . . . H23A H -1.2542 0.6260 -0.9819 0.108 Uiso 1 1 calc R . . C24 C -1.2666(3) 0.5352(6) -1.0626(3) 0.095(3) Uani 1 1 d . . . H24A H -1.2970 0.5894 -1.0819 0.114 Uiso 1 1 calc R . . C25 C -1.2054(2) 0.3703(6) -1.0644(3) 0.087(2) Uani 1 1 d . . . H25A H -1.1915 0.3056 -1.0857 0.104 Uiso 1 1 calc R . . C26 C -1.1778(2) 0.3865(7) -1.0042(3) 0.084(2) Uani 1 1 d . . . H26A H -1.1469 0.3327 -0.9859 0.100 Uiso 1 1 calc R . . C27 C -1.3923(2) 1.3166(5) -0.5672(3) 0.079(2) Uani 1 1 d . . . H27A H -1.3810 1.3689 -0.5322 0.095 Uiso 1 1 calc R . . C28 C -1.3531(3) 1.2603(5) -0.5926(3) 0.083(2) Uani 1 1 d . . . H28A H -1.3156 1.2789 -0.5748 0.100 Uiso 1 1 calc R . . C29 C -1.4214(3) 1.1616(6) -0.6660(3) 0.083(2) Uani 1 1 d . . . H29A H -1.4316 1.1087 -0.7009 0.099 Uiso 1 1 calc R . . C30 C -1.4634(3) 1.2115(5) -0.6454(3) 0.078(2) Uani 1 1 d . . . H30A H -1.5006 1.1915 -0.6645 0.094 Uiso 1 1 calc R . . C31 C -1.4477(3) 1.2934(5) -0.5945(3) 0.0670(19) Uani 1 1 d . . . C32 C -1.4906(3) 1.3514(6) -0.5705(3) 0.077(2) Uani 1 1 d . . . H32A H -1.4802 1.4159 -0.5398 0.093 Uiso 1 1 calc R . . C34 C -1.6506(2) 1.3694(6) -0.5183(3) 0.0687(17) Uani 1 1 d . . . C33 C -1.6062(2) 1.3087(5) -0.5396(3) 0.0628(18) Uani 1 1 d . . . C35 C -1.6904(3) 1.4523(6) -0.5556(3) 0.089(2) Uani 1 1 d . . . H35A H -1.6886 1.4733 -0.5942 0.107 Uiso 1 1 calc R . . C36 C -1.7334(3) 1.5042(6) -0.5352(3) 0.102(3) Uani 1 1 d . . . H36A H -1.7606 1.5591 -0.5604 0.123 Uiso 1 1 calc R . . C37 C -1.7359(3) 1.4741(6) -0.4768(3) 0.102(3) Uani 1 1 d . . . H37A H -1.7643 1.5096 -0.4628 0.123 Uiso 1 1 calc R . . C38 C -1.6968(3) 1.3935(6) -0.4413(3) 0.095(2) Uani 1 1 d . . . H38A H -1.6984 1.3728 -0.4026 0.114 Uiso 1 1 calc R . . C39 C -1.6544(3) 1.3408(5) -0.4615(3) 0.081(2) Uani 1 1 d . . . H39A H -1.6279 1.2848 -0.4361 0.098 Uiso 1 1 calc R . . C40 C -1.5985(2) 1.1565(5) -0.5341(3) 0.0621(18) Uani 1 1 d . . . C41 C -1.6404(3) 1.0751(5) -0.5759(3) 0.073(2) Uani 1 1 d . . . C42 C -1.6709(3) 1.1266(7) -0.6299(3) 0.097(2) Uani 1 1 d U . . H42A H -1.6641 1.2155 -0.6398 0.116 Uiso 1 1 calc R . . C43 C -1.7121(3) 1.0510(7) -0.6711(4) 0.134(3) Uani 1 1 d U . . H43A H -1.7320 1.0871 -0.7083 0.161 Uiso 1 1 calc R . . C44 C -1.7219(3) 0.9231(8) -0.6546(4) 0.144(4) Uani 1 1 d . . . H44A H -1.7497 0.8726 -0.6814 0.173 Uiso 1 1 calc R . . C45 C -1.6937(3) 0.8643(8) -0.6017(4) 0.134(3) Uani 1 1 d U . . H45A H -1.7017 0.7760 -0.5923 0.161 Uiso 1 1 calc R . . C46 C -1.6515(3) 0.9420(6) -0.5611(3) 0.100(2) Uani 1 1 d . . . H46A H -1.6312 0.9043 -0.5245 0.120 Uiso 1 1 calc R . . C47 C -1.4886(2) 1.1211(6) -0.4121(3) 0.075(2) Uani 1 1 d . . . H47A H -1.4912 1.0265 -0.4122 0.090 Uiso 1 1 calc R . . C48 C -1.4457(2) 1.1822(5) -0.3640(3) 0.0647(18) Uani 1 1 d . . . C49 C -1.4166(2) 1.1054(6) -0.3153(3) 0.079(2) Uani 1 1 d . . . H49A H -1.4248 1.0134 -0.3134 0.095 Uiso 1 1 calc R . . C50 C -1.3752(2) 1.1640(6) -0.2692(3) 0.073(2) Uani 1 1 d . . . H50A H -1.3560 1.1098 -0.2369 0.087 Uiso 1 1 calc R . . C51 C -1.3901(2) 1.3686(6) -0.3177(3) 0.073(2) Uani 1 1 d . . . H51A H -1.3811 1.4601 -0.3195 0.088 Uiso 1 1 calc R . . C52 C -1.4315(3) 1.3164(6) -0.3646(3) 0.081(2) Uani 1 1 d . . . H52A H -1.4499 1.3719 -0.3967 0.097 Uiso 1 1 calc R . . S1 S -1.20942(9) 1.55741(19) -0.66333(10) 0.1231(8) Uani 1 1 d U . . C53 C -1.2415(3) 1.4127(6) -0.6666(3) 0.081(2) Uani 1 1 d U . . N13 N -1.2636(2) 1.3104(4) -0.6696(2) 0.0744(17) Uani 1 1 d . . . S2 S -1.41298(12) 0.7129(2) -0.71021(11) 0.1653(11) Uani 1 1 d U . . C54 C -1.3714(3) 0.8414(6) -0.7055(3) 0.099(2) Uani 1 1 d U . . N14 N -1.3416(2) 0.9299(4) -0.7013(2) 0.0814(17) Uani 1 1 d . . . N15 N -1.1232(8) 1.4336(15) -0.4822(8) 0.226(7) Uiso 0.50 1 d PDU A 1 C55 C -1.1175(11) 1.5388(15) -0.5075(11) 0.194(5) Uiso 0.50 1 d PDU A 1 C56 C -1.1168(9) 1.6895(14) -0.5214(9) 0.202(7) Uiso 0.50 1 d PDU A 1 H56A H -1.1539 1.7194 -0.5418 0.303 Uiso 0.50 1 calc PR A 1 H56B H -1.0930 1.7052 -0.5467 0.303 Uiso 0.50 1 calc PR A 1 H56C H -1.1029 1.7394 -0.4843 0.303 Uiso 0.50 1 calc PR A 1 N15' N -1.1079(7) 1.4200(14) -0.5104(8) 0.199(6) Uiso 0.50 1 d PDU B 2 C55' C -1.1216(12) 1.5354(15) -0.5019(13) 0.192(5) Uiso 0.50 1 d PDU B 2 C56' C -1.1368(9) 1.6852(15) -0.5056(10) 0.203(7) Uiso 0.50 1 d PDU B 2 H56D H -1.1752 1.6950 -0.5065 0.304 Uiso 0.50 1 calc PR B 2 H56E H -1.1314 1.7235 -0.5417 0.304 Uiso 0.50 1 calc PR B 2 H56F H -1.1135 1.7318 -0.4710 0.304 Uiso 0.50 1 calc PR B 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 Zn1 0.0787(5) 0.0632(4) 0.0878(5) -0.0036(5) 0.0338(4) 0.0010(5) C1 0.089(4) 0.077(4) 0.181(6) -0.036(4) 0.088(4) -0.015(4) N1 0.077(3) 0.060(3) 0.104(4) 0.000(3) 0.042(3) 0.012(3) C2 0.098(5) 0.061(4) 0.135(6) 0.003(4) 0.054(4) -0.017(4) N2 0.091(4) 0.069(3) 0.136(5) -0.006(3) 0.059(3) 0.006(3) C3 0.119(5) 0.063(4) 0.141(6) 0.019(4) 0.069(5) 0.013(4) N3 0.093(4) 0.068(3) 0.124(4) 0.000(3) 0.061(3) 0.002(3) C4 0.134(5) 0.075(5) 0.131(5) 0.012(4) 0.088(4) 0.019(4) N4 0.069(3) 0.077(3) 0.099(4) -0.009(3) 0.034(3) -0.013(3) C5 0.068(4) 0.081(4) 0.099(5) -0.008(4) 0.040(4) -0.003(4) N5 0.076(4) 0.095(4) 0.078(4) -0.007(3) 0.014(3) -0.007(3) C6 0.090(5) 0.068(4) 0.102(5) -0.002(4) 0.050(4) -0.010(4) N6 0.070(3) 0.067(3) 0.100(4) 0.007(3) 0.048(3) 0.012(3) N7 0.064(3) 0.067(3) 0.088(4) -0.009(3) 0.039(3) -0.004(3) N8 0.077(3) 0.063(3) 0.101(4) 0.002(3) 0.053(3) 0.001(3) N9 0.076(3) 0.060(3) 0.094(4) 0.003(3) 0.038(3) -0.003(3) C7 0.063(4) 0.075(4) 0.114(5) -0.006(4) 0.048(4) -0.006(4) C8 0.085(4) 0.083(4) 0.101(4) 0.003(4) 0.044(4) 0.003(4) C9 0.094(5) 0.092(4) 0.133(5) -0.003(4) 0.054(4) 0.008(4) C10 0.116(5) 0.113(5) 0.141(5) -0.004(4) 0.054(4) 0.024(4) C11 0.152(6) 0.146(6) 0.168(6) 0.001(5) 0.094(5) 0.032(5) C12 0.178(6) 0.182(6) 0.192(6) 0.025(6) 0.119(5) 0.020(6) C13 0.158(6) 0.136(6) 0.171(6) 0.027(5) 0.097(5) 0.027(5) N10 0.086(4) 0.064(3) 0.073(3) -0.005(3) 0.015(3) -0.008(3) N11 0.082(4) 0.079(3) 0.068(4) 0.006(3) 0.015(3) 0.012(3) N12 0.069(3) 0.057(3) 0.076(3) 0.000(3) 0.035(3) -0.013(3) C14 0.069(4) 0.077(4) 0.088(5) -0.015(4) 0.043(4) 0.006(4) C15 0.076(4) 0.071(4) 0.086(5) -0.008(4) 0.038(4) 0.014(4) C16 0.113(6) 0.132(6) 0.104(6) -0.007(5) 0.044(5) -0.010(5) C17 0.166(8) 0.157(7) 0.073(5) 0.001(5) 0.030(6) -0.011(7) C18 0.167(8) 0.138(7) 0.128(7) -0.015(6) 0.050(6) 0.033(7) C19 0.114(7) 0.116(6) 0.111(7) -0.040(5) -0.006(6) 0.007(6) C20 0.089(5) 0.085(5) 0.121(6) -0.029(5) 0.037(5) -0.001(5) C21 0.075(5) 0.080(4) 0.090(5) -0.005(4) 0.036(4) -0.006(4) C22 0.070(5) 0.088(4) 0.088(5) 0.001(4) 0.037(4) 0.003(4) C23 0.087(5) 0.082(4) 0.095(5) -0.016(4) 0.015(4) 0.014(4) C24 0.084(5) 0.082(5) 0.113(6) -0.009(5) 0.015(5) 0.009(4) C25 0.062(4) 0.094(5) 0.102(5) -0.032(4) 0.020(4) 0.007(4) C26 0.060(4) 0.101(5) 0.094(5) -0.002(5) 0.030(4) 0.021(4) C27 0.074(5) 0.070(4) 0.086(5) -0.023(4) 0.012(4) -0.015(4) C28 0.080(5) 0.072(4) 0.102(5) -0.024(4) 0.032(4) -0.008(4) C29 0.073(4) 0.091(5) 0.092(5) -0.023(4) 0.037(4) -0.020(4) C30 0.065(4) 0.085(4) 0.095(5) -0.009(4) 0.040(4) -0.014(4) C31 0.074(4) 0.050(3) 0.081(5) -0.007(3) 0.030(4) -0.003(4) C32 0.088(5) 0.063(4) 0.093(5) -0.001(3) 0.044(4) -0.006(4) C34 0.074(4) 0.057(3) 0.090(4) -0.009(3) 0.047(3) -0.012(4) C33 0.064(4) 0.058(4) 0.069(4) -0.006(3) 0.025(3) -0.012(3) C35 0.084(5) 0.088(4) 0.103(5) -0.002(4) 0.041(4) 0.012(4) C36 0.071(5) 0.090(5) 0.144(7) -0.002(5) 0.028(5) 0.011(4) C37 0.095(5) 0.095(5) 0.137(6) -0.022(5) 0.065(5) -0.002(4) C38 0.104(5) 0.083(4) 0.116(5) -0.010(5) 0.059(4) -0.016(5) C39 0.086(5) 0.063(4) 0.115(5) -0.005(4) 0.060(4) -0.009(4) C40 0.077(4) 0.049(4) 0.070(4) -0.002(3) 0.036(3) 0.001(3) C41 0.080(5) 0.057(4) 0.089(5) -0.009(3) 0.032(4) 0.008(4) C42 0.101(5) 0.077(4) 0.100(5) -0.022(4) 0.010(4) 0.014(4) C43 0.126(6) 0.135(5) 0.141(6) -0.037(5) 0.037(5) 0.033(5) C44 0.131(7) 0.137(7) 0.175(8) -0.087(6) 0.061(6) -0.014(6) C45 0.137(6) 0.107(5) 0.167(6) -0.033(5) 0.056(5) -0.030(5) C46 0.108(6) 0.093(5) 0.106(6) -0.021(4) 0.043(5) -0.021(5) C47 0.070(4) 0.069(4) 0.084(5) -0.004(4) 0.020(4) -0.005(4) C48 0.069(4) 0.059(4) 0.067(4) 0.009(3) 0.021(3) 0.005(3) C49 0.088(5) 0.051(3) 0.100(5) 0.008(4) 0.029(4) 0.003(4) C50 0.074(5) 0.063(4) 0.076(4) 0.011(3) 0.014(4) 0.003(4) C51 0.096(5) 0.056(3) 0.069(4) 0.013(4) 0.027(4) 0.006(4) C52 0.095(5) 0.063(4) 0.081(5) 0.006(4) 0.019(4) -0.002(4) S1 0.1406(18) 0.1084(14) 0.1296(17) -0.0178(13) 0.0536(14) -0.0501(14) C53 0.099(4) 0.072(4) 0.081(4) -0.014(3) 0.041(3) -0.001(4) N13 0.076(4) 0.061(3) 0.084(4) -0.014(3) 0.020(3) -0.003(3) S2 0.195(2) 0.1422(18) 0.139(2) 0.0005(17) 0.0180(19) -0.0864(19) C54 0.130(5) 0.092(4) 0.082(4) -0.010(4) 0.041(4) -0.037(4) N14 0.081(4) 0.070(3) 0.104(4) 0.000(3) 0.044(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N14 2.072(5) . ? Zn1 N13 2.108(5) . ? Zn1 N6 2.210(5) 4_576 ? Zn1 N12 2.216(4) 4_585 ? Zn1 N1 2.221(5) . ? Zn1 N7 2.232(5) . ? C1 C5 1.348(8) . ? C1 C2 1.377(8) . ? C1 H1A 0.9300 . ? N1 C3 1.330(7) . ? N1 C2 1.356(6) . ? C2 H2A 0.9300 . ? N2 C6 1.254(6) . ? N2 N3 1.411(6) . ? C3 C4 1.366(8) . ? C3 H3A 0.9300 . ? N3 C7 1.286(7) . ? C4 C5 1.379(7) . ? C4 H4A 0.9300 . ? N4 C14 1.278(7) . ? N4 N5 1.378(6) . ? C5 C6 1.441(8) . ? N5 C21 1.256(7) . ? C6 H6A 0.9300 . ? N6 C25 1.328(7) . ? N6 C24 1.336(7) . ? N6 Zn1 2.210(5) 4_575 ? N7 C28 1.314(7) . ? N7 C29 1.330(7) . ? N8 C32 1.257(7) . ? N8 N9 1.399(6) . ? N9 C33 1.274(6) . ? C7 C8 1.473(8) . ? C7 C14 1.513(8) . ? C8 C13 1.355(9) . ? C8 C9 1.387(8) . ? C9 C10 1.413(9) . ? C9 H9A 0.9300 . ? C10 C11 1.307(10) . ? C10 H10A 0.9300 . ? C11 C12 1.347(10) . ? C11 H11A 0.9300 . ? C12 C13 1.419(10) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? N10 C40 1.278(6) . ? N10 N11 1.391(6) . ? N11 C47 1.263(6) . ? N12 C51 1.340(6) . ? N12 C50 1.353(6) . ? N12 Zn1 2.216(4) 4_586 ? C14 C15 1.475(8) . ? C15 C16 1.390(9) . ? C15 C20 1.403(8) . ? C16 C17 1.367(9) . ? C16 H16A 0.9300 . ? C17 C18 1.372(10) . ? C17 H17A 0.9300 . ? C18 C19 1.414(10) . ? C18 H18A 0.9300 . ? C19 C20 1.377(9) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.441(8) . ? C21 H21A 0.9300 . ? C22 C23 1.352(8) . ? C22 C26 1.383(8) . ? C23 C24 1.382(8) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.374(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C31 1.367(7) . ? C27 C28 1.396(8) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 C30 1.365(7) . ? C29 H29A 0.9300 . ? C30 C31 1.385(7) . ? C30 H30A 0.9300 . ? C31 C32 1.461(8) . ? C32 H32A 0.9300 . ? C34 C39 1.373(7) . ? C34 C35 1.380(7) . ? C34 C33 1.466(7) . ? C33 C40 1.507(7) . ? C35 C36 1.392(8) . ? C35 H35A 0.9300 . ? C36 C37 1.399(9) . ? C36 H36A 0.9300 . ? C37 C38 1.339(8) . ? C37 H37A 0.9300 . ? C38 C39 1.379(8) . ? C38 H38A 0.9300 . ? C39 H39A 0.9300 . ? C40 C41 1.444(7) . ? C41 C42 1.359(8) . ? C41 C46 1.399(7) . ? C42 C43 1.399(9) . ? C42 H42A 0.9300 . ? C43 C44 1.355(10) . ? C43 H43A 0.9300 . ? C44 C45 1.353(10) . ? C44 H44A 0.9300 . ? C45 C46 1.415(9) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 C48 1.437(7) . ? C47 H47A 0.9300 . ? C48 C52 1.365(7) . ? C48 C49 1.376(7) . ? C49 C50 1.380(7) . ? C49 H49A 0.9300 . ? C50 H50A 0.9300 . ? C51 C52 1.365(7) . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? S1 C53 1.623(6) . ? C53 N13 1.140(6) . ? S2 C54 1.621(7) . ? C54 N14 1.131(7) . ? N15 C55 1.215(16) . ? C55 C56 1.515(14) . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? N15' C55' 1.216(15) . ? C55' C56' 1.515(15) . ? C56' H56D 0.9600 . ? C56' H56E 0.9600 . ? C56' H56F 0.9600 . ? 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 N14 Zn1 N13 179.5(2) . . ? N14 Zn1 N6 93.18(18) . 4_576 ? N13 Zn1 N6 86.59(17) . 4_576 ? N14 Zn1 N12 91.39(18) . 4_585 ? N13 Zn1 N12 88.89(17) . 4_585 ? N6 Zn1 N12 171.02(16) 4_576 4_585 ? N14 Zn1 N1 90.14(18) . . ? N13 Zn1 N1 89.45(18) . . ? N6 Zn1 N1 92.17(17) 4_576 . ? N12 Zn1 N1 95.54(17) 4_585 . ? N14 Zn1 N7 88.33(18) . . ? N13 Zn1 N7 92.07(18) . . ? N6 Zn1 N7 86.93(17) 4_576 . ? N12 Zn1 N7 85.49(16) 4_585 . ? N1 Zn1 N7 178.18(17) . . ? C5 C1 C2 121.0(6) . . ? C5 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? C3 N1 C2 114.5(5) . . ? C3 N1 Zn1 124.6(4) . . ? C2 N1 Zn1 120.9(4) . . ? N1 C2 C1 122.9(6) . . ? N1 C2 H2A 118.6 . . ? C1 C2 H2A 118.6 . . ? C6 N2 N3 113.9(5) . . ? N1 C3 C4 125.6(6) . . ? N1 C3 H3A 117.2 . . ? C4 C3 H3A 117.2 . . ? C7 N3 N2 111.8(5) . . ? C3 C4 C5 118.7(6) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C14 N4 N5 118.0(5) . . ? C1 C5 C4 117.3(6) . . ? C1 C5 C6 121.8(6) . . ? C4 C5 C6 120.8(6) . . ? C21 N5 N4 118.8(6) . . ? N2 C6 C5 122.0(6) . . ? N2 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C25 N6 C24 114.5(5) . . ? C25 N6 Zn1 123.7(4) . 4_575 ? C24 N6 Zn1 121.0(4) . 4_575 ? C28 N7 C29 116.7(5) . . ? C28 N7 Zn1 120.2(4) . . ? C29 N7 Zn1 122.2(4) . . ? C32 N8 N9 117.5(5) . . ? C33 N9 N8 115.6(5) . . ? N3 C7 C8 119.2(6) . . ? N3 C7 C14 122.8(6) . . ? C8 C7 C14 118.0(5) . . ? C13 C8 C9 117.3(7) . . ? C13 C8 C7 120.9(6) . . ? C9 C8 C7 121.8(6) . . ? C8 C9 C10 121.4(7) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 119.5(7) . . ? C11 C10 H10A 120.3 . . ? C9 C10 H10A 120.3 . . ? C10 C11 C12 121.2(9) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C11 C12 C13 120.5(9) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C8 C13 C12 120.1(8) . . ? C8 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C40 N10 N11 114.3(4) . . ? C47 N11 N10 112.3(5) . . ? C51 N12 C50 115.5(5) . . ? C51 N12 Zn1 126.4(4) . 4_586 ? C50 N12 Zn1 117.5(4) . 4_586 ? N4 C14 C15 120.3(6) . . ? N4 C14 C7 121.4(6) . . ? C15 C14 C7 118.3(5) . . ? C16 C15 C20 118.1(6) . . ? C16 C15 C14 119.5(6) . . ? C20 C15 C14 122.3(6) . . ? C17 C16 C15 119.0(7) . . ? C17 C16 H16A 120.5 . . ? C15 C16 H16A 120.5 . . ? C16 C17 C18 124.7(9) . . ? C16 C17 H17A 117.6 . . ? C18 C17 H17A 117.6 . . ? C17 C18 C19 116.2(8) . . ? C17 C18 H18A 121.9 . . ? C19 C18 H18A 121.9 . . ? C20 C19 C18 120.3(8) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C15 121.5(7) . . ? C19 C20 H20A 119.2 . . ? C15 C20 H20A 119.2 . . ? N5 C21 C22 123.0(6) . . ? N5 C21 H21A 118.5 . . ? C22 C21 H21A 118.5 . . ? C23 C22 C26 115.8(6) . . ? C23 C22 C21 123.6(6) . . ? C26 C22 C21 120.5(6) . . ? C22 C23 C24 121.6(6) . . ? C22 C23 H23A 119.2 . . ? C24 C23 H23A 119.2 . . ? N6 C24 C23 123.3(6) . . ? N6 C24 H24A 118.4 . . ? C23 C24 H24A 118.4 . . ? N6 C25 C26 125.4(6) . . ? N6 C25 H25A 117.3 . . ? C26 C25 H25A 117.3 . . ? C25 C26 C22 119.4(6) . . ? C25 C26 H26A 120.3 . . ? C22 C26 H26A 120.3 . . ? C31 C27 C28 118.9(6) . . ? C31 C27 H27A 120.6 . . ? C28 C27 H27A 120.6 . . ? N7 C28 C27 122.6(6) . . ? N7 C28 H28A 118.7 . . ? C27 C28 H28A 118.7 . . ? N7 C29 C30 125.9(6) . . ? N7 C29 H29A 117.1 . . ? C30 C29 H29A 117.1 . . ? C29 C30 C31 116.4(6) . . ? C29 C30 H30A 121.8 . . ? C31 C30 H30A 121.8 . . ? C27 C31 C30 119.4(6) . . ? C27 C31 C32 121.3(6) . . ? C30 C31 C32 119.3(6) . . ? N8 C32 C31 122.5(6) . . ? N8 C32 H32A 118.8 . . ? C31 C32 H32A 118.8 . . ? C39 C34 C35 118.7(6) . . ? C39 C34 C33 120.5(5) . . ? C35 C34 C33 120.8(6) . . ? N9 C33 C34 118.9(5) . . ? N9 C33 C40 123.1(5) . . ? C34 C33 C40 117.8(5) . . ? C34 C35 C36 119.7(6) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C35 C36 C37 120.2(7) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? C38 C37 C36 119.2(7) . . ? C38 C37 H37A 120.4 . . ? C36 C37 H37A 120.4 . . ? C37 C38 C39 120.8(7) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C34 C39 C38 121.4(6) . . ? C34 C39 H39A 119.3 . . ? C38 C39 H39A 119.3 . . ? N10 C40 C41 118.8(5) . . ? N10 C40 C33 124.8(5) . . ? C41 C40 C33 116.3(5) . . ? C42 C41 C46 118.2(6) . . ? C42 C41 C40 121.0(5) . . ? C46 C41 C40 120.8(6) . . ? C41 C42 C43 122.5(7) . . ? C41 C42 H42A 118.7 . . ? C43 C42 H42A 118.7 . . ? C44 C43 C42 117.2(8) . . ? C44 C43 H43A 121.4 . . ? C42 C43 H43A 121.4 . . ? C45 C44 C43 124.1(8) . . ? C45 C44 H44A 118.0 . . ? C43 C44 H44A 118.0 . . ? C44 C45 C46 117.7(8) . . ? C44 C45 H45A 121.2 . . ? C46 C45 H45A 121.2 . . ? C41 C46 C45 120.3(7) . . ? C41 C46 H46A 119.8 . . ? C45 C46 H46A 119.8 . . ? N11 C47 C48 125.9(6) . . ? N11 C47 H47A 117.0 . . ? C48 C47 H47A 117.0 . . ? C52 C48 C49 117.3(6) . . ? C52 C48 C47 122.3(6) . . ? C49 C48 C47 120.4(5) . . ? C48 C49 C50 120.4(5) . . ? C48 C49 H49A 119.8 . . ? C50 C49 H49A 119.8 . . ? N12 C50 C49 122.5(5) . . ? N12 C50 H50A 118.8 . . ? C49 C50 H50A 118.8 . . ? N12 C51 C52 124.6(5) . . ? N12 C51 H51A 117.7 . . ? C52 C51 H51A 117.7 . . ? C51 C52 C48 119.7(6) . . ? C51 C52 H52A 120.2 . . ? C48 C52 H52A 120.2 . . ? N13 C53 S1 178.8(7) . . ? C53 N13 Zn1 173.1(5) . . ? N14 C54 S2 178.7(7) . . ? C54 N14 Zn1 164.6(5) . . ? N15 C55 C56 160(3) . . ? N15' C55' C56' 167(3) . . ? C55' C56' H56D 109.5 . . ? C55' C56' H56E 109.5 . . ? H56D C56' H56E 109.5 . . ? C55' C56' H56F 109.5 . . ? H56D C56' H56F 109.5 . . ? H56E C56' H56F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.291 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.045 # Attachment '5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 748794' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H20 Ag N7 O3' _chemical_formula_sum 'C26 H20 Ag N7 O3' _chemical_formula_weight 586.36 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 10.380(6) _cell_length_b 11.008(7) _cell_length_c 11.174(7) _cell_angle_alpha 105.477(10) _cell_angle_beta 91.417(11) _cell_angle_gamma 103.155(10) _cell_volume 1193.2(13) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3256 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 22.67 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6079 _diffrn_reflns_av_R_equivalents 0.0116 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4139 _reflns_number_gt 3490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; To assist the refinement,the thermal parameters on adjacent atoms in NO~3~^-^ anion were restrained to be similar. 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^)+(0.0406P)^2^+0.6482P] 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 4139 _refine_ls_number_parameters 334 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.180 _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 -0.36124(3) 0.83988(3) 0.98140(3) 0.06606(13) Uani 1 1 d . . . N1 N -0.1793(2) 0.8906(2) 0.8913(2) 0.0426(6) Uani 1 1 d . . . N2 N 0.0279(2) 0.6162(2) 0.7186(2) 0.0412(6) Uani 1 1 d . . . N3 N 0.1074(2) 0.5422(2) 0.6477(2) 0.0396(5) Uani 1 1 d . . . N4 N 0.0323(2) 0.3840(2) 0.8536(2) 0.0388(5) Uani 1 1 d . . . N5 N 0.1641(2) 0.4540(2) 0.8906(2) 0.0411(6) Uani 1 1 d . . . N6 N 0.5250(2) 0.6987(3) 1.0661(2) 0.0479(6) Uani 1 1 d . . . C1 C -0.1266(3) 1.0132(3) 0.8968(3) 0.0446(7) Uani 1 1 d . . . H1A H -0.1701 1.0760 0.9361 0.053 Uiso 1 1 calc R . . C2 C -0.0108(3) 1.0513(3) 0.8470(3) 0.0476(7) Uani 1 1 d . . . H2A H 0.0227 1.1384 0.8513 0.057 Uiso 1 1 calc R . . C3 C 0.0556(3) 0.9612(3) 0.7907(3) 0.0448(7) Uani 1 1 d . . . H3A H 0.1349 0.9859 0.7566 0.054 Uiso 1 1 calc R . . C4 C -0.1149(3) 0.8035(3) 0.8363(3) 0.0405(7) Uani 1 1 d . . . H4A H -0.1519 0.7169 0.8319 0.049 Uiso 1 1 calc R . . C5 C 0.0036(3) 0.8327(3) 0.7852(3) 0.0364(6) Uani 1 1 d . . . C6 C 0.0714(3) 0.7344(3) 0.7254(3) 0.0385(6) Uani 1 1 d . . . H6A H 0.1500 0.7596 0.6906 0.046 Uiso 1 1 calc R . . C7 C 0.0892(3) 0.4276(3) 0.6572(2) 0.0343(6) Uani 1 1 d . . . C8 C 0.1636(3) 0.3417(3) 0.5796(3) 0.0382(6) Uani 1 1 d . . . C9 C 0.2596(3) 0.3901(3) 0.5093(3) 0.0493(8) Uani 1 1 d . . . H9A H 0.2786 0.4777 0.5123 0.059 Uiso 1 1 calc R . . C10 C 0.3271(3) 0.3093(4) 0.4349(3) 0.0591(9) Uani 1 1 d . . . H10A H 0.3915 0.3427 0.3880 0.071 Uiso 1 1 calc R . . C11 C 0.3007(4) 0.1814(4) 0.4293(3) 0.0616(10) Uani 1 1 d . . . H11A H 0.3464 0.1272 0.3785 0.074 Uiso 1 1 calc R . . C12 C 0.2079(4) 0.1330(4) 0.4979(4) 0.0637(10) Uani 1 1 d . . . H12A H 0.1903 0.0454 0.4945 0.076 Uiso 1 1 calc R . . C13 C 0.1384(3) 0.2127(3) 0.5733(3) 0.0509(8) Uani 1 1 d . . . H13A H 0.0743 0.1782 0.6198 0.061 Uiso 1 1 calc R . . C14 C -0.0039(3) 0.3738(3) 0.7405(3) 0.0348(6) Uani 1 1 d . . . C15 C -0.1391(3) 0.3003(3) 0.6888(3) 0.0374(6) Uani 1 1 d . . . C16 C -0.1892(3) 0.3046(3) 0.5755(3) 0.0500(8) Uani 1 1 d . . . H16A H -0.1378 0.3560 0.5319 0.060 Uiso 1 1 calc R . . C17 C -0.3156(4) 0.2328(4) 0.5260(4) 0.0655(10) Uani 1 1 d . . . H17A H -0.3494 0.2358 0.4492 0.079 Uiso 1 1 calc R . . C18 C -0.3903(3) 0.1579(3) 0.5903(4) 0.0662(11) Uani 1 1 d . . . H18A H -0.4752 0.1093 0.5568 0.079 Uiso 1 1 calc R . . C19 C -0.3421(3) 0.1531(3) 0.7032(4) 0.0597(10) Uani 1 1 d . . . H19A H -0.3939 0.1013 0.7463 0.072 Uiso 1 1 calc R . . C20 C -0.2169(3) 0.2249(3) 0.7531(3) 0.0461(7) Uani 1 1 d . . . H20A H -0.1845 0.2226 0.8306 0.055 Uiso 1 1 calc R . . C21 C 0.1934(3) 0.4701(3) 1.0044(3) 0.0397(6) Uani 1 1 d . . . H21A H 0.1299 0.4350 1.0511 0.048 Uiso 1 1 calc R . . C22 C 0.3247(3) 0.5425(3) 1.0647(3) 0.0390(6) Uani 1 1 d . . . C23 C 0.3709(3) 0.5295(3) 1.1758(3) 0.0488(8) Uani 1 1 d . . . H23A H 0.3183 0.4734 1.2144 0.059 Uiso 1 1 calc R . . C24 C 0.4945(4) 0.5996(3) 1.2292(3) 0.0560(9) Uani 1 1 d . . . H24A H 0.5276 0.5908 1.3037 0.067 Uiso 1 1 calc R . . C25 C 0.5679(3) 0.6818(3) 1.1724(3) 0.0544(8) Uani 1 1 d . . . H25A H 0.6523 0.7287 1.2090 0.065 Uiso 1 1 calc R . . C26 C 0.4060(3) 0.6286(3) 1.0136(3) 0.0438(7) Uani 1 1 d . . . H26A H 0.3760 0.6382 0.9383 0.053 Uiso 1 1 calc R . . N7 N -0.5947(3) 0.9016(4) 0.8424(4) 0.0753(8) Uani 1 1 d U . . O1 O -0.6309(4) 0.9058(4) 0.9462(3) 0.1068(10) Uani 1 1 d U . . O2 O -0.6271(3) 0.9733(3) 0.7880(3) 0.0906(9) Uani 1 1 d U . . O3 O -0.5282(3) 0.8281(3) 0.7960(3) 0.0911(8) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04754(17) 0.0744(2) 0.0722(2) 0.01897(15) 0.02022(13) 0.00721(13) N1 0.0416(13) 0.0436(15) 0.0451(14) 0.0129(11) 0.0082(11) 0.0141(11) N2 0.0448(13) 0.0368(14) 0.0456(14) 0.0120(11) 0.0149(11) 0.0152(11) N3 0.0444(13) 0.0366(13) 0.0393(14) 0.0092(11) 0.0124(11) 0.0135(11) N4 0.0382(12) 0.0389(13) 0.0372(14) 0.0094(10) 0.0042(10) 0.0067(10) N5 0.0401(13) 0.0449(14) 0.0343(14) 0.0086(11) 0.0025(10) 0.0052(11) N6 0.0388(14) 0.0533(16) 0.0450(15) 0.0037(12) 0.0064(12) 0.0092(12) C1 0.0528(18) 0.0418(17) 0.0454(17) 0.0134(14) 0.0071(14) 0.0223(14) C2 0.0563(19) 0.0321(15) 0.0571(19) 0.0156(14) 0.0085(15) 0.0124(14) C3 0.0438(16) 0.0397(16) 0.0516(18) 0.0161(14) 0.0096(14) 0.0071(13) C4 0.0430(16) 0.0330(15) 0.0440(17) 0.0106(13) 0.0057(13) 0.0062(12) C5 0.0389(15) 0.0334(14) 0.0358(15) 0.0082(12) 0.0041(12) 0.0082(12) C6 0.0423(15) 0.0363(16) 0.0379(16) 0.0106(12) 0.0093(12) 0.0106(12) C7 0.0346(14) 0.0351(15) 0.0313(14) 0.0055(12) 0.0020(11) 0.0095(11) C8 0.0394(15) 0.0422(16) 0.0319(15) 0.0035(12) 0.0014(12) 0.0161(12) C9 0.0496(18) 0.058(2) 0.0477(18) 0.0189(15) 0.0132(14) 0.0227(15) C10 0.053(2) 0.084(3) 0.048(2) 0.0176(18) 0.0172(16) 0.0339(19) C11 0.064(2) 0.075(3) 0.047(2) -0.0021(18) 0.0052(17) 0.043(2) C12 0.073(2) 0.049(2) 0.069(2) 0.0041(18) 0.009(2) 0.0302(18) C13 0.0547(19) 0.0441(18) 0.054(2) 0.0080(15) 0.0115(15) 0.0187(15) C14 0.0372(14) 0.0297(14) 0.0379(16) 0.0062(12) 0.0077(12) 0.0123(11) C15 0.0371(14) 0.0306(14) 0.0419(16) 0.0034(12) 0.0063(12) 0.0108(11) C16 0.0437(17) 0.059(2) 0.0404(17) 0.0047(15) 0.0024(14) 0.0101(15) C17 0.051(2) 0.075(3) 0.053(2) -0.0072(19) -0.0049(17) 0.0131(18) C18 0.0390(18) 0.048(2) 0.089(3) -0.014(2) -0.0021(19) 0.0046(15) C19 0.0429(18) 0.0336(17) 0.100(3) 0.0144(18) 0.0187(19) 0.0088(14) C20 0.0424(16) 0.0356(16) 0.065(2) 0.0181(15) 0.0114(15) 0.0132(13) C21 0.0458(16) 0.0354(15) 0.0377(17) 0.0102(12) 0.0052(13) 0.0094(12) C22 0.0470(16) 0.0356(15) 0.0320(15) 0.0032(12) 0.0034(12) 0.0130(13) C23 0.063(2) 0.0426(17) 0.0402(17) 0.0099(14) -0.0003(15) 0.0134(15) C24 0.065(2) 0.060(2) 0.0402(18) 0.0070(16) -0.0092(16) 0.0198(18) C25 0.0445(18) 0.059(2) 0.049(2) -0.0019(16) -0.0047(15) 0.0138(16) C26 0.0465(17) 0.0481(17) 0.0354(16) 0.0074(13) 0.0041(13) 0.0143(14) N7 0.0603(15) 0.0936(18) 0.0731(16) 0.0086(15) 0.0126(13) 0.0377(13) O1 0.115(2) 0.114(2) 0.090(2) 0.0165(18) 0.0420(18) 0.0355(19) O2 0.0698(17) 0.090(2) 0.107(2) 0.0246(17) -0.0030(16) 0.0147(15) O3 0.0775(16) 0.112(2) 0.0802(16) 0.0003(15) 0.0102(13) 0.0485(14) _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 N6 2.170(3) 1_455 ? Ag1 N1 2.192(3) . ? Ag1 O3 2.625(3) . ? Ag1 O1 2.720(4) 2_477 ? N1 C4 1.320(4) . ? N1 C1 1.320(4) . ? N2 C6 1.257(4) . ? N2 N3 1.402(3) . ? N3 C7 1.266(4) . ? N4 C14 1.278(4) . ? N4 N5 1.399(3) . ? N5 C21 1.255(4) . ? N6 C26 1.324(4) . ? N6 C25 1.332(4) . ? N6 Ag1 2.170(3) 1_655 ? C1 C2 1.363(5) . ? C1 H1A 0.9300 . ? C2 C3 1.362(4) . ? C2 H2A 0.9300 . ? C3 C5 1.378(4) . ? C3 H3A 0.9300 . ? C4 C5 1.377(4) . ? C4 H4A 0.9300 . ? C5 C6 1.448(4) . ? C6 H6A 0.9300 . ? C7 C8 1.473(4) . ? C7 C14 1.493(4) . ? C8 C13 1.366(4) . ? C8 C9 1.384(4) . ? C9 C10 1.375(5) . ? C9 H9A 0.9300 . ? C10 C11 1.356(6) . ? C10 H10A 0.9300 . ? C11 C12 1.349(6) . ? C11 H11A 0.9300 . ? C12 C13 1.387(5) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.466(4) . ? C15 C16 1.374(4) . ? C15 C20 1.378(4) . ? C16 C17 1.383(5) . ? C16 H16A 0.9300 . ? C17 C18 1.360(6) . ? C17 H17A 0.9300 . ? C18 C19 1.365(6) . ? C18 H18A 0.9300 . ? C19 C20 1.373(5) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.456(4) . ? C21 H21A 0.9300 . ? C22 C26 1.373(4) . ? C22 C23 1.375(4) . ? C23 C24 1.365(5) . ? C23 H23A 0.9300 . ? C24 C25 1.349(5) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? N7 O3 1.203(4) . ? N7 O2 1.213(5) . ? N7 O1 1.221(5) . ? 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 N6 Ag1 N1 144.32(10) 1_455 . ? N6 Ag1 O3 102.24(11) 1_455 . ? N1 Ag1 O3 96.55(11) . . ? N6 Ag1 O1 121.80(11) 1_455 2_477 ? N1 Ag1 O1 90.07(10) . 2_477 ? O3 Ag1 O1 83.48(11) . 2_477 ? C4 N1 C1 117.6(3) . . ? C4 N1 Ag1 122.4(2) . . ? C1 N1 Ag1 119.8(2) . . ? C6 N2 N3 110.2(2) . . ? C7 N3 N2 114.7(2) . . ? C14 N4 N5 113.2(2) . . ? C21 N5 N4 111.5(2) . . ? C26 N6 C25 117.7(3) . . ? C26 N6 Ag1 119.6(2) . 1_655 ? C25 N6 Ag1 122.6(2) . 1_655 ? N1 C1 C2 122.5(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 119.7(3) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C5 118.9(3) . . ? C2 C3 H3A 120.5 . . ? C5 C3 H3A 120.5 . . ? N1 C4 C5 124.1(3) . . ? N1 C4 H4A 118.0 . . ? C5 C4 H4A 118.0 . . ? C4 C5 C3 117.1(3) . . ? C4 C5 C6 122.5(3) . . ? C3 C5 C6 120.3(3) . . ? N2 C6 C5 122.5(3) . . ? N2 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 . . ? N3 C7 C8 117.6(3) . . ? N3 C7 C14 124.2(2) . . ? C8 C7 C14 118.2(2) . . ? C13 C8 C9 118.4(3) . . ? C13 C8 C7 121.2(3) . . ? C9 C8 C7 120.3(3) . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 120.7(3) . . ? C11 C10 H10A 119.7 . . ? C9 C10 H10A 119.7 . . ? C12 C11 C10 119.7(3) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 120.6(4) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C8 C13 C12 120.3(3) . . ? C8 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? N4 C14 C15 118.8(2) . . ? N4 C14 C7 122.1(2) . . ? C15 C14 C7 119.0(2) . . ? C16 C15 C20 119.2(3) . . ? C16 C15 C14 120.6(3) . . ? C20 C15 C14 120.3(3) . . ? C15 C16 C17 120.3(3) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 120.8(3) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C19 C20 C15 120.3(3) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? N5 C21 C22 121.4(3) . . ? N5 C21 H21A 119.3 . . ? C22 C21 H21A 119.3 . . ? C26 C22 C23 117.5(3) . . ? C26 C22 C21 121.0(3) . . ? C23 C22 C21 121.5(3) . . ? C24 C23 C22 119.5(3) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C25 C24 C23 119.1(3) . . ? C25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? N6 C25 C24 122.9(3) . . ? N6 C25 H25A 118.6 . . ? C24 C25 H25A 118.6 . . ? N6 C26 C22 123.3(3) . . ? N6 C26 H26A 118.3 . . ? C22 C26 H26A 118.3 . . ? O3 N7 O2 121.2(4) . . ? O3 N7 O1 120.4(4) . . ? O2 N7 O1 118.4(4) . . ? N7 O3 Ag1 104.1(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.655 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.055 # Attachment '6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 748795' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H40 Cl2 Fe N12, C2 H3 N' _chemical_formula_sum 'C54 H43 Cl2 Fe N13' _chemical_formula_weight 1000.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 8.5305(8) _cell_length_b 10.6074(10) _cell_length_c 14.4874(13) _cell_angle_alpha 92.912(2) _cell_angle_beta 92.474(2) _cell_angle_gamma 104.149(2) _cell_volume 1267.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 642 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 19.03 _exptl_crystal_description orange _exptl_crystal_colour block _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 518 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6856 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.1457 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4673 _reflns_number_gt 2287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The half CH~3~CN molecule is considered disordered in which the N(7) and C(27) atoms are disordered over two positions in the refined ratio 0.25:0.25. It was refined with bond distances and anisotropic displacement parameters restraints. 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^)+(0.0330P)^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 4673 _refine_ls_number_parameters 351 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1641 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.036 _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 Fe1 Fe -0.5000 -0.5000 -0.5000 0.03405(16) Uani 1 2 d S . . Cl1 Cl -0.75455(8) -0.54110(6) -0.59256(4) 0.0475(2) Uani 1 1 d . . . N1 N -0.5842(2) -0.34649(18) -0.40789(13) 0.0379(6) Uani 1 1 d . . . N2 N -0.4162(2) -0.01774(18) -0.16282(13) 0.0387(7) Uani 1 1 d . . . N3 N -0.3047(2) 0.01856(18) -0.08523(13) 0.0358(6) Uani 1 1 d . . . N4 N -0.2149(2) 0.28756(19) -0.19987(13) 0.0418(7) Uani 1 1 d . . . N5 N -0.0771(3) 0.23827(19) -0.21446(14) 0.0441(7) Uani 1 1 d . . . N6 N 0.3792(2) 0.35524(18) -0.40321(13) 0.0395(7) Uani 1 1 d . . . C1 C -0.4966(3) -0.2922(2) -0.33014(17) 0.0441(9) Uani 1 1 d . . . H1A H -0.4054 -0.3211 -0.3135 0.053 Uiso 1 1 calc R . . C2 C -0.7202(3) -0.3081(2) -0.42461(18) 0.0508(9) Uani 1 1 d . . . H2A H -0.7846 -0.3443 -0.4774 0.061 Uiso 1 1 calc R . . C3 C -0.7711(4) -0.2197(3) -0.36974(19) 0.0614(10) Uani 1 1 d . . . H3A H -0.8690 -0.1993 -0.3840 0.074 Uiso 1 1 calc R . . C4 C -0.6766(3) -0.1615(2) -0.29368(18) 0.0512(9) Uani 1 1 d . . . H4A H -0.7081 -0.0995 -0.2561 0.061 Uiso 1 1 calc R . . C5 C -0.5341(3) -0.1956(2) -0.27316(17) 0.0390(8) Uani 1 1 d . . . C6 C -0.4238(3) -0.1331(2) -0.19387(16) 0.0439(9) Uani 1 1 d . . . H6A H -0.3578 -0.1798 -0.1657 0.053 Uiso 1 1 calc R . . C7 C -0.2528(3) 0.1415(2) -0.06935(15) 0.0306(7) Uani 1 1 d . . . C8 C -0.1474(3) 0.1900(2) 0.01557(16) 0.0334(7) Uani 1 1 d . . . C9 C -0.1004(3) 0.3220(2) 0.04172(18) 0.0483(9) Uani 1 1 d . . . H9A H -0.1322 0.3809 0.0042 0.058 Uiso 1 1 calc R . . C10 C -0.0067(3) 0.3676(3) 0.12289(18) 0.0587(10) Uani 1 1 d . . . H10A H 0.0248 0.4564 0.1396 0.070 Uiso 1 1 calc R . . C11 C 0.0391(3) 0.2795(3) 0.17835(19) 0.0588(10) Uani 1 1 d . . . H11A H 0.1000 0.3094 0.2334 0.071 Uiso 1 1 calc R . . C12 C -0.0042(3) 0.1472(3) 0.15336(18) 0.0545(10) Uani 1 1 d . . . H12A H 0.0291 0.0884 0.1904 0.065 Uiso 1 1 calc R . . C13 C -0.0975(3) 0.1046(3) 0.07258(16) 0.0437(9) Uani 1 1 d . . . H13A H -0.1280 0.0158 0.0558 0.052 Uiso 1 1 calc R . . C14 C -0.2961(3) 0.2407(2) -0.13073(16) 0.0317(7) Uani 1 1 d . . . C15 C -0.4344(3) 0.2940(2) -0.10761(16) 0.0334(8) Uani 1 1 d . . . C16 C -0.5516(3) 0.2298(2) -0.05198(17) 0.0395(8) Uani 1 1 d . . . H16A H -0.5411 0.1534 -0.0266 0.047 Uiso 1 1 calc R . . C17 C -0.6851(3) 0.2783(2) -0.03348(18) 0.0505(9) Uani 1 1 d . . . H17A H -0.7640 0.2341 0.0036 0.061 Uiso 1 1 calc R . . C18 C -0.6995(3) 0.3910(3) -0.07015(18) 0.0533(9) Uani 1 1 d . . . H18A H -0.7887 0.4233 -0.0575 0.064 Uiso 1 1 calc R . . C19 C -0.5850(3) 0.4577(2) -0.12540(19) 0.0546(10) Uani 1 1 d . . . H19A H -0.5970 0.5343 -0.1501 0.065 Uiso 1 1 calc R . . C20 C -0.4522(3) 0.4106(2) -0.14409(18) 0.0467(9) Uani 1 1 d . . . H20A H -0.3738 0.4560 -0.1810 0.056 Uiso 1 1 calc R . . C21 C -0.0001(3) 0.2974(2) -0.27994(17) 0.0444(9) Uani 1 1 d . . . H21A H -0.0449 0.3568 -0.3101 0.053 Uiso 1 1 calc R . . C22 C 0.1530(3) 0.2776(2) -0.31014(16) 0.0373(8) Uani 1 1 d . . . C23 C 0.2273(3) 0.1854(2) -0.27532(17) 0.0461(9) Uani 1 1 d . . . H23A H 0.1765 0.1280 -0.2331 0.055 Uiso 1 1 calc R . . C24 C 0.3772(3) 0.1808(2) -0.30454(17) 0.0443(9) Uani 1 1 d . . . H24A H 0.4294 0.1201 -0.2824 0.053 Uiso 1 1 calc R . . C25 C 0.4482(3) 0.2668(2) -0.36655(17) 0.0466(9) Uani 1 1 d . . . H25A H 0.5507 0.2640 -0.3845 0.056 Uiso 1 1 calc R . . C26 C 0.2309(3) 0.3568(2) -0.37416(16) 0.0408(8) Uani 1 1 d . . . H26A H 0.1787 0.4156 -0.3994 0.049 Uiso 1 1 calc R . . N7 N 0.8813(7) -0.1455(6) -0.4535(5) 0.052(3) Uani 0.25 1 d PD A 1 C27 C 0.8200(7) -0.0592(6) -0.4356(8) 0.054(3) Uani 0.25 1 d PDU A 1 C28 C 0.7096(5) 0.0141(4) -0.4266(4) 0.075(2) Uani 0.50 1 d PD A 1 H28A H 0.7293 0.0810 -0.4699 0.113 Uiso 0.50 1 calc PR A 1 H28B H 0.7197 0.0534 -0.3648 0.113 Uiso 0.50 1 calc PR A 1 H28C H 0.6023 -0.0405 -0.4389 0.113 Uiso 0.50 1 calc PR A 1 N7' N 0.8757(8) -0.1326(5) -0.3908(6) 0.062(3) Uani 0.25 1 d PDU B 2 C27' C 0.8407(8) -0.0323(6) -0.3992(9) 0.081(4) Uani 0.25 1 d PDU B 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 Fe1 0.0375(3) 0.0349(3) 0.0288(3) 0.0000(2) 0.0056(2) 0.0069(3) Cl1 0.0458(4) 0.0556(4) 0.0404(4) -0.0069(3) -0.0030(3) 0.0140(3) N1 0.0383(13) 0.0378(11) 0.0362(12) -0.0035(10) -0.0005(10) 0.0082(10) N2 0.0444(13) 0.0317(11) 0.0372(12) -0.0052(9) -0.0030(10) 0.0062(10) N3 0.0383(13) 0.0359(11) 0.0320(12) -0.0015(9) 0.0023(10) 0.0079(10) N4 0.0413(13) 0.0450(12) 0.0420(13) 0.0103(10) 0.0126(10) 0.0132(11) N5 0.0421(13) 0.0491(12) 0.0441(13) 0.0114(11) 0.0162(11) 0.0130(11) N6 0.0399(13) 0.0380(11) 0.0433(13) 0.0047(10) 0.0063(10) 0.0138(10) C1 0.0446(17) 0.0375(14) 0.0487(17) -0.0068(13) -0.0052(14) 0.0107(13) C2 0.0485(18) 0.0550(17) 0.0488(17) -0.0096(14) -0.0050(15) 0.0166(15) C3 0.0542(18) 0.0681(18) 0.067(2) -0.0182(16) -0.0081(16) 0.0314(15) C4 0.0491(18) 0.0495(16) 0.0554(18) -0.0136(14) 0.0029(15) 0.0162(14) C5 0.0409(16) 0.0345(14) 0.0397(16) -0.0015(12) 0.0055(13) 0.0060(13) C6 0.0573(18) 0.0390(15) 0.0373(16) -0.0006(13) 0.0012(14) 0.0164(14) C7 0.0320(14) 0.0322(13) 0.0294(14) 0.0039(11) 0.0094(11) 0.0093(11) C8 0.0331(15) 0.0356(13) 0.0320(14) -0.0027(11) 0.0006(12) 0.0105(12) C9 0.0525(18) 0.0408(15) 0.0509(17) 0.0003(13) -0.0074(14) 0.0127(14) C10 0.063(2) 0.0430(17) 0.062(2) -0.0154(15) -0.0060(16) 0.0035(16) C11 0.0477(19) 0.083(2) 0.0401(17) -0.0044(16) -0.0030(14) 0.0076(17) C12 0.0505(19) 0.0662(18) 0.0456(17) 0.0172(15) -0.0040(15) 0.0106(16) C13 0.0445(17) 0.0488(16) 0.0352(15) 0.0065(13) 0.0028(13) 0.0060(14) C14 0.0328(15) 0.0278(13) 0.0318(14) 0.0024(11) 0.0054(12) 0.0017(12) C15 0.0354(15) 0.0305(13) 0.0346(14) 0.0031(11) 0.0019(12) 0.0084(12) C16 0.0412(16) 0.0357(14) 0.0448(16) 0.0044(12) 0.0086(13) 0.0142(13) C17 0.0473(17) 0.0535(17) 0.0545(18) 0.0073(14) 0.0192(14) 0.0161(14) C18 0.0498(17) 0.0574(17) 0.0581(18) -0.0083(15) 0.0062(15) 0.0256(14) C19 0.0630(19) 0.0387(15) 0.069(2) 0.0080(14) 0.0057(16) 0.0254(14) C20 0.0428(17) 0.0367(15) 0.0593(18) 0.0071(14) 0.0047(14) 0.0061(14) C21 0.0425(17) 0.0465(15) 0.0437(16) 0.0130(13) 0.0113(13) 0.0065(14) C22 0.0423(16) 0.0368(14) 0.0314(15) 0.0113(12) 0.0082(12) 0.0045(13) C23 0.0441(18) 0.0416(15) 0.0466(17) 0.0112(13) 0.0058(14) -0.0032(14) C24 0.0456(17) 0.0432(15) 0.0468(17) 0.0141(13) 0.0034(14) 0.0136(13) C25 0.0395(16) 0.0510(16) 0.0528(18) 0.0057(14) 0.0062(14) 0.0167(14) C26 0.0397(16) 0.0477(15) 0.0378(16) 0.0084(13) 0.0044(13) 0.0147(13) N7 0.028(5) 0.085(7) 0.030(5) 0.008(5) -0.004(4) -0.008(5) C27 0.055(5) 0.038(5) 0.067(5) -0.005(4) 0.030(4) 0.004(4) C28 0.089(5) 0.096(4) 0.053(4) 0.053(3) 0.021(3) 0.033(4) N7' 0.040(4) 0.094(5) 0.057(5) 0.015(4) -0.014(4) 0.030(4) C27' 0.092(6) 0.070(6) 0.071(6) -0.013(5) 0.019(5) 0.004(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 Fe1 N6 2.2262(19) 1_445 ? Fe1 N6 2.2262(19) 2_554 ? Fe1 N1 2.320(2) . ? Fe1 N1 2.320(2) 2_444 ? Fe1 Cl1 2.4351(7) 2_444 ? Fe1 Cl1 2.4351(7) . ? N1 C2 1.337(3) . ? N1 C1 1.345(3) . ? N2 C6 1.268(3) . ? N2 N3 1.414(2) . ? N3 C7 1.276(3) . ? N4 C14 1.293(3) . ? N4 N5 1.418(3) . ? N5 C21 1.280(3) . ? N6 C25 1.342(3) . ? N6 C26 1.354(3) . ? N6 Fe1 2.2262(19) 1_665 ? C1 C5 1.390(3) . ? C1 H1A 0.9300 . ? C2 C3 1.361(4) . ? C2 H2A 0.9300 . ? C3 C4 1.362(3) . ? C3 H3A 0.9300 . ? C4 C5 1.375(4) . ? C4 H4A 0.9300 . ? C5 C6 1.473(3) . ? C6 H6A 0.9300 . ? C7 C8 1.484(3) . ? C7 C14 1.514(3) . ? C8 C13 1.385(3) . ? C8 C9 1.386(3) . ? C9 C10 1.389(3) . ? C9 H9A 0.9300 . ? C10 C11 1.378(4) . ? C10 H10A 0.9300 . ? C11 C12 1.386(4) . ? C11 H11A 0.9300 . ? C12 C13 1.378(3) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.471(4) . ? C15 C16 1.380(3) . ? C15 C20 1.408(3) . ? C16 C17 1.389(4) . ? C16 H16A 0.9300 . ? C17 C18 1.363(4) . ? C17 H17A 0.9300 . ? C18 C19 1.372(4) . ? C18 H18A 0.9300 . ? C19 C20 1.377(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.455(4) . ? C21 H21A 0.9300 . ? C22 C26 1.367(3) . ? C22 C23 1.392(4) . ? C23 C24 1.375(4) . ? C23 H23A 0.9300 . ? C24 C25 1.366(3) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? N7 C27 1.183(7) . ? C27 C28 1.366(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? N7' C27' 1.184(7) . ? 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 N6 Fe1 N6 180.00 1_445 2_554 ? N6 Fe1 N1 86.20(7) 1_445 . ? N6 Fe1 N1 93.80(7) 2_554 . ? N6 Fe1 N1 93.80(7) 1_445 2_444 ? N6 Fe1 N1 86.20(7) 2_554 2_444 ? N1 Fe1 N1 180.00 . 2_444 ? N6 Fe1 Cl1 91.06(5) 1_445 2_444 ? N6 Fe1 Cl1 88.94(5) 2_554 2_444 ? N1 Fe1 Cl1 90.73(5) . 2_444 ? N1 Fe1 Cl1 89.27(5) 2_444 2_444 ? N6 Fe1 Cl1 88.94(5) 1_445 . ? N6 Fe1 Cl1 91.06(5) 2_554 . ? N1 Fe1 Cl1 89.27(5) . . ? N1 Fe1 Cl1 90.73(5) 2_444 . ? Cl1 Fe1 Cl1 180.0 2_444 . ? C2 N1 C1 115.3(2) . . ? C2 N1 Fe1 124.54(15) . . ? C1 N1 Fe1 120.13(17) . . ? C6 N2 N3 111.2(2) . . ? C7 N3 N2 113.76(19) . . ? C14 N4 N5 114.1(2) . . ? C21 N5 N4 108.7(2) . . ? C25 N6 C26 115.8(2) . . ? C25 N6 Fe1 123.72(17) . 1_665 ? C26 N6 Fe1 120.38(16) . 1_665 ? N1 C1 C5 123.9(3) . . ? N1 C1 H1A 118.0 . . ? C5 C1 H1A 118.0 . . ? N1 C2 C3 124.6(2) . . ? N1 C2 H2A 117.7 . . ? C3 C2 H2A 117.7 . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C4 C5 C1 117.7(2) . . ? C4 C5 C6 121.9(2) . . ? C1 C5 C6 120.4(2) . . ? N2 C6 C5 122.0(2) . . ? N2 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? N3 C7 C8 118.0(2) . . ? N3 C7 C14 123.8(2) . . ? C8 C7 C14 118.08(19) . . ? C13 C8 C9 118.1(2) . . ? C13 C8 C7 121.0(2) . . ? C9 C8 C7 120.9(2) . . ? C8 C9 C10 121.2(2) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C11 C10 C9 119.1(2) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 121.0(2) . . ? C10 C11 H11A 119.5 . . ? C12 C11 H11A 119.5 . . ? C13 C12 C11 118.6(3) . . ? C13 C12 H12A 120.7 . . ? C11 C12 H12A 120.7 . . ? C12 C13 C8 122.0(2) . . ? C12 C13 H13A 119.0 . . ? C8 C13 H13A 119.0 . . ? N4 C14 C15 117.0(2) . . ? N4 C14 C7 124.6(2) . . ? C15 C14 C7 118.3(2) . . ? C16 C15 C20 118.4(2) . . ? C16 C15 C14 121.2(2) . . ? C20 C15 C14 120.4(2) . . ? C15 C16 C17 120.8(2) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 119.5(3) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 121.4(3) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C18 C19 C20 119.6(3) . . ? C18 C19 H19A 120.2 . . ? C20 C19 H19A 120.2 . . ? C19 C20 C15 120.4(2) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? N5 C21 C22 124.1(3) . . ? N5 C21 H21A 118.0 . . ? C22 C21 H21A 118.0 . . ? C26 C22 C23 118.1(3) . . ? C26 C22 C21 118.1(2) . . ? C23 C22 C21 123.8(2) . . ? C24 C23 C22 118.8(2) . . ? C24 C23 H23A 120.6 . . ? C22 C23 H23A 120.6 . . ? C25 C24 C23 119.0(3) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? N6 C25 C24 124.1(3) . . ? N6 C25 H25A 118.0 . . ? C24 C25 H25A 118.0 . . ? N6 C26 C22 124.2(2) . . ? N6 C26 H26A 117.9 . . ? C22 C26 H26A 117.9 . . ? N7 C27 C28 162.9(7) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.648 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.070 # Attachment '7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 748796' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H46 Mn N14 O S2' _chemical_formula_weight 1050.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4934(14) _cell_length_b 10.3652(17) _cell_length_c 14.878(2) _cell_angle_alpha 85.775(3) _cell_angle_beta 84.341(3) _cell_angle_gamma 79.168(3) _cell_volume 1428.6(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1090 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 22.47 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.221 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 545 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7330 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0853 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4989 _reflns_number_gt 2857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The one half EtOH molecule is rotationally disordered over two orientations in the refined ratio 0.25:0.25. It was refined with distance and anisotropic displacement parameters restraints. C-C bonds were restrained to 1.48 \%A. C-O bonds were restrained to 1.40 \%A. The distance of the two terminal atoms of CH~3~CN molecule was restrained to 2.88 \%A. 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^)+(0.0862P)^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 4989 _refine_ls_number_parameters 377 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1640 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.056 _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 Mn1 Mn 0.0000 1.0000 0.5000 0.04388(17) Uani 1 2 d S . . N1 N 0.1279(2) 0.8570(2) 0.39670(15) 0.0527(7) Uani 1 1 d . . . N2 N 0.5710(3) 0.7463(2) 0.20851(17) 0.0654(8) Uani 1 1 d . . . N3 N 0.7019(3) 0.7929(2) 0.19547(17) 0.0633(8) Uani 1 1 d . . . N4 N 0.7924(2) 0.5157(2) 0.08689(15) 0.0506(7) Uani 1 1 d . . . N5 N 0.8892(3) 0.4811(2) 0.15467(16) 0.0524(7) Uani 1 1 d . . . N6 N 1.0436(2) 0.1712(2) 0.39269(15) 0.0504(7) Uani 1 1 d . . . C1 C 0.2647(3) 0.8611(3) 0.36766(19) 0.0555(9) Uani 1 1 d . . . H1A H 0.3100 0.9189 0.3942 0.067 Uiso 1 1 calc R . . C2 C 0.0652(4) 0.7726(3) 0.3578(2) 0.0673(10) Uani 1 1 d . . . H2A H -0.0303 0.7687 0.3766 0.081 Uiso 1 1 calc R . . C3 C 0.1343(4) 0.6912(3) 0.2912(2) 0.0798(12) Uani 1 1 d . . . H3A H 0.0866 0.6334 0.2666 0.096 Uiso 1 1 calc R . . C4 C 0.2765(4) 0.6973(3) 0.2619(2) 0.0742(11) Uani 1 1 d . . . H4A H 0.3255 0.6437 0.2172 0.089 Uiso 1 1 calc R . . C5 C 0.3444(3) 0.7846(3) 0.3002(2) 0.0581(9) Uani 1 1 d . . . C6 C 0.4900(3) 0.8046(3) 0.2729(2) 0.0638(10) Uani 1 1 d . . . H6A H 0.5269 0.8634 0.3042 0.077 Uiso 1 1 calc R . . C7 C 0.7873(3) 0.7432(3) 0.12970(19) 0.0493(8) Uani 1 1 d . . . C8 C 0.9231(3) 0.7932(3) 0.10651(19) 0.0509(8) Uani 1 1 d . . . C9 C 0.9424(4) 0.9087(3) 0.1418(2) 0.0728(11) Uani 1 1 d . . . H9A H 0.8692 0.9553 0.1793 0.087 Uiso 1 1 calc R . . C10 C 1.0702(4) 0.9540(3) 0.1212(3) 0.0879(13) Uani 1 1 d . . . H10A H 1.0834 1.0305 0.1456 0.106 Uiso 1 1 calc R . . C11 C 1.1793(4) 0.8857(3) 0.0640(3) 0.0815(12) Uani 1 1 d . . . H11A H 1.2650 0.9168 0.0499 0.098 Uiso 1 1 calc R . . C12 C 1.1604(3) 0.7736(3) 0.0290(2) 0.0674(10) Uani 1 1 d . . . H12A H 1.2334 0.7280 -0.0091 0.081 Uiso 1 1 calc R . . C13 C 1.0345(3) 0.7271(3) 0.0494(2) 0.0582(9) Uani 1 1 d . . . H13A H 1.0231 0.6502 0.0247 0.070 Uiso 1 1 calc R . . C14 C 0.7503(3) 0.6406(3) 0.07300(18) 0.0454(8) Uani 1 1 d . . . C15 C 0.6602(3) 0.6866(3) -0.00329(19) 0.0491(8) Uani 1 1 d . . . C16 C 0.6214(4) 0.8199(3) -0.0270(2) 0.0743(11) Uani 1 1 d . . . H16A H 0.6511 0.8811 0.0062 0.089 Uiso 1 1 calc R . . C17 C 0.5398(4) 0.8632(4) -0.0987(3) 0.0923(13) Uani 1 1 d . . . H17A H 0.5164 0.9528 -0.1139 0.111 Uiso 1 1 calc R . . C18 C 0.4933(4) 0.7762(4) -0.1471(2) 0.0873(13) Uani 1 1 d . . . H18A H 0.4366 0.8066 -0.1945 0.105 Uiso 1 1 calc R . . C19 C 0.5301(3) 0.6405(4) -0.1263(2) 0.0749(11) Uani 1 1 d . . . H19A H 0.4992 0.5803 -0.1597 0.090 Uiso 1 1 calc R . . C20 C 0.6139(3) 0.5981(3) -0.0543(2) 0.0610(9) Uani 1 1 d . . . H20A H 0.6394 0.5084 -0.0400 0.073 Uiso 1 1 calc R . . C21 C 0.8825(3) 0.3706(3) 0.1949(2) 0.0551(9) Uani 1 1 d . . . H21A H 0.8124 0.3244 0.1825 0.066 Uiso 1 1 calc R . . C22 C 0.9866(3) 0.3146(3) 0.26189(19) 0.0471(8) Uani 1 1 d . . . C23 C 1.1167(3) 0.3552(3) 0.2597(2) 0.0620(9) Uani 1 1 d . . . H23A H 1.1422 0.4162 0.2150 0.074 Uiso 1 1 calc R . . C24 C 1.2081(3) 0.3044(3) 0.3243(2) 0.0731(11) Uani 1 1 d . . . H24A H 1.2974 0.3293 0.3236 0.088 Uiso 1 1 calc R . . C25 C 1.1660(3) 0.2160(3) 0.3903(2) 0.0600(9) Uani 1 1 d . . . H25A H 1.2267 0.1859 0.4357 0.072 Uiso 1 1 calc R . . C26 C 0.9557(3) 0.2213(3) 0.32802(19) 0.0537(8) Uani 1 1 d . . . H26A H 0.8694 0.1912 0.3280 0.064 Uiso 1 1 calc R . . N7 N 0.1968(2) 1.0055(2) 0.55869(16) 0.0552(7) Uani 1 1 d . . . C27 C 0.3081(3) 0.9542(3) 0.58116(19) 0.0499(8) Uani 1 1 d . . . S1 S 0.46103(11) 0.87841(12) 0.61188(8) 0.1015(4) Uani 1 1 d . . . O1 O 0.2493(15) 0.4130(12) 0.5846(10) 0.158(5) Uani 0.25 1 d PDU A 1 H1B H 0.2293 0.3886 0.5370 0.237 Uiso 0.25 1 calc PR A 1 C28 C 0.3189(19) 0.5267(16) 0.5660(12) 0.152(6) Uani 0.25 1 d PDU A 1 H28A H 0.2492 0.5948 0.5383 0.183 Uiso 0.25 1 calc PR A 1 H28B H 0.3964 0.5022 0.5194 0.183 Uiso 0.25 1 calc PR A 1 C29 C 0.382(3) 0.593(3) 0.6362(17) 0.245(7) Uani 0.25 1 d PDU A 1 H29A H 0.3676 0.6861 0.6220 0.367 Uiso 0.25 1 calc PR A 1 H29B H 0.4835 0.5586 0.6360 0.367 Uiso 0.25 1 calc PR A 1 H29C H 0.3356 0.5759 0.6950 0.367 Uiso 0.25 1 calc PR A 1 O1' O 0.2271(16) 0.5175(16) 0.5183(9) 0.166(5) Uani 0.25 1 d PDU B 2 H1'A H 0.1841 0.4650 0.4992 0.250 Uiso 0.25 1 calc PR B 2 C28' C 0.3022(18) 0.4576(18) 0.5918(11) 0.136(6) Uani 0.25 1 d PDU B 2 H28C H 0.3624 0.3773 0.5709 0.164 Uiso 0.25 1 calc PR B 2 H28D H 0.2311 0.4313 0.6374 0.164 Uiso 0.25 1 calc PR B 2 C29' C 0.395(2) 0.527(2) 0.6391(14) 0.158(6) Uani 0.25 1 d PDU B 2 H29D H 0.4471 0.4659 0.6815 0.237 Uiso 0.25 1 calc PR B 2 H29E H 0.3365 0.5978 0.6708 0.237 Uiso 0.25 1 calc PR B 2 H29F H 0.4625 0.5609 0.5955 0.237 Uiso 0.25 1 calc PR B 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 Mn1 0.0275(3) 0.0475(3) 0.0499(4) 0.0108(3) -0.0027(3) 0.0049(3) N1 0.0416(13) 0.0518(14) 0.0586(15) 0.0031(11) 0.0041(12) 0.0006(11) N2 0.0553(15) 0.0671(16) 0.0656(16) -0.0044(13) 0.0105(13) 0.0021(13) N3 0.0508(15) 0.0647(16) 0.0676(16) -0.0108(13) 0.0108(13) 0.0009(13) N4 0.0474(13) 0.0418(12) 0.0569(14) 0.0110(10) -0.0050(12) 0.0016(11) N5 0.0474(13) 0.0422(13) 0.0602(15) 0.0123(11) -0.0076(12) 0.0061(11) N6 0.0365(12) 0.0473(13) 0.0628(15) 0.0164(11) -0.0067(11) -0.0023(10) C1 0.0468(17) 0.0557(17) 0.0592(19) -0.0027(14) 0.0025(15) -0.0014(14) C2 0.0542(18) 0.0586(19) 0.086(2) -0.0009(17) -0.0020(18) -0.0056(16) C3 0.079(2) 0.062(2) 0.099(3) -0.0182(18) 0.000(2) -0.0108(18) C4 0.076(2) 0.062(2) 0.075(2) -0.0112(17) 0.0053(19) 0.0080(18) C5 0.0541(18) 0.0561(18) 0.0550(19) 0.0005(15) 0.0051(15) 0.0069(15) C6 0.0566(19) 0.0633(19) 0.063(2) -0.0072(15) 0.0097(16) 0.0048(16) C7 0.0480(16) 0.0426(15) 0.0497(17) 0.0021(13) 0.0014(14) 0.0067(13) C8 0.0468(16) 0.0410(15) 0.0580(18) 0.0006(13) 0.0016(14) 0.0051(13) C9 0.062(2) 0.0546(19) 0.096(2) -0.0120(17) -0.0015(19) 0.0035(17) C10 0.080(2) 0.054(2) 0.133(3) -0.005(2) -0.016(2) -0.0175(18) C11 0.061(2) 0.069(2) 0.111(3) 0.0101(19) 0.004(2) -0.0158(18) C12 0.0547(19) 0.0583(19) 0.082(2) 0.0040(16) 0.0124(17) -0.0055(16) C13 0.0537(18) 0.0465(16) 0.069(2) 0.0006(14) 0.0088(16) -0.0041(15) C14 0.0383(15) 0.0417(15) 0.0485(16) 0.0058(12) 0.0058(13) 0.0042(12) C15 0.0418(15) 0.0470(15) 0.0515(17) 0.0125(13) -0.0038(14) 0.0038(13) C16 0.082(2) 0.0481(18) 0.085(2) 0.0121(16) -0.021(2) 0.0084(17) C17 0.098(3) 0.069(2) 0.099(3) 0.030(2) -0.030(2) 0.012(2) C18 0.056(2) 0.117(3) 0.074(2) 0.033(2) -0.0119(18) 0.010(2) C19 0.0532(19) 0.101(3) 0.069(2) 0.0084(19) -0.0140(17) -0.0120(19) C20 0.0523(18) 0.0605(18) 0.065(2) 0.0094(16) -0.0040(16) -0.0013(15) C21 0.0503(17) 0.0490(16) 0.0643(19) 0.0131(14) -0.0097(15) -0.0084(14) C22 0.0435(16) 0.0376(14) 0.0556(17) 0.0099(12) -0.0077(14) 0.0011(12) C23 0.0495(18) 0.0514(17) 0.076(2) 0.0280(15) -0.0003(16) 0.0003(14) C24 0.0372(16) 0.075(2) 0.102(3) 0.0359(18) -0.0105(17) -0.0100(15) C25 0.0367(16) 0.0646(19) 0.073(2) 0.0229(16) -0.0101(15) -0.0016(14) C26 0.0472(16) 0.0500(16) 0.0639(19) 0.0178(14) -0.0139(15) -0.0118(14) N7 0.0370(13) 0.0646(15) 0.0597(15) 0.0121(12) -0.0072(12) -0.0026(11) C27 0.0363(15) 0.0614(17) 0.0498(17) 0.0096(13) -0.0064(13) -0.0065(14) S1 0.0521(5) 0.1183(8) 0.1246(9) 0.0301(7) -0.0364(6) 0.0097(6) O1 0.166(7) 0.171(7) 0.150(7) -0.014(6) -0.040(6) -0.046(6) C28 0.146(8) 0.151(9) 0.160(9) -0.028(7) 0.000(7) -0.028(7) C29 0.243(10) 0.241(10) 0.245(10) 0.003(7) -0.011(7) -0.040(7) O1' 0.182(8) 0.153(7) 0.154(7) -0.016(6) -0.038(6) 0.010(6) C28' 0.137(8) 0.132(8) 0.134(9) 0.005(7) -0.014(7) -0.013(7) C29' 0.160(9) 0.150(9) 0.155(9) 0.014(7) -0.005(7) -0.018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N7 2.151(2) 2_576 ? Mn1 N7 2.151(2) . ? Mn1 N1 2.308(2) 2_576 ? Mn1 N1 2.308(2) . ? Mn1 N6 2.366(2) 2_666 ? Mn1 N6 2.366(2) 1_465 ? N1 C1 1.335(4) . ? N1 C2 1.339(4) . ? N2 C6 1.280(4) . ? N2 N3 1.407(4) . ? N3 C7 1.281(3) . ? N4 C14 1.289(3) . ? N4 N5 1.413(3) . ? N5 C21 1.261(3) . ? N6 C25 1.327(4) . ? N6 C26 1.346(3) . ? N6 Mn1 2.366(2) 1_645 ? C1 C5 1.396(4) . ? C1 H1A 0.9300 . ? C2 C3 1.382(5) . ? C2 H2A 0.9300 . ? C3 C4 1.388(5) . ? C3 H3A 0.9300 . ? C4 C5 1.389(5) . ? C4 H4A 0.9300 . ? C5 C6 1.450(4) . ? C6 H6A 0.9300 . ? C7 C8 1.478(4) . ? C7 C14 1.515(4) . ? C8 C9 1.392(4) . ? C8 C13 1.395(4) . ? C9 C10 1.380(5) . ? C9 H9A 0.9300 . ? C10 C11 1.392(5) . ? C10 H10A 0.9300 . ? C11 C12 1.356(5) . ? C11 H11A 0.9300 . ? C12 C13 1.370(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.485(4) . ? C15 C20 1.389(4) . ? C15 C16 1.390(4) . ? C16 C17 1.379(5) . ? C16 H16A 0.9300 . ? C17 C18 1.354(6) . ? C17 H17A 0.9300 . ? C18 C19 1.403(5) . ? C18 H18A 0.9300 . ? C19 C20 1.393(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.483(4) . ? C21 H21A 0.9300 . ? C22 C23 1.374(4) . ? C22 C26 1.378(4) . ? C23 C24 1.369(4) . ? C23 H23A 0.9300 . ? C24 C25 1.375(4) . ? C24 H24A 0.9300 . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? N7 C27 1.159(3) . ? C27 S1 1.607(3) . ? O1 C28 1.453(15) . ? O1 H1B 0.8200 . ? C28 C29 1.520(17) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O1' C28' 1.406(15) . ? O1' H1'A 0.8200 . ? C28' C29' 1.492(17) . ? C28' H28C 0.9700 . ? C28' H28D 0.9700 . ? C29' H29D 0.9600 . ? C29' H29E 0.9600 . ? C29' H29F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Mn1 N7 180.0 2_576 . ? N7 Mn1 N1 89.37(9) 2_576 2_576 ? N7 Mn1 N1 90.63(9) . 2_576 ? N7 Mn1 N1 90.63(9) 2_576 . ? N7 Mn1 N1 89.37(9) . . ? N1 Mn1 N1 180.0 2_576 . ? N7 Mn1 N6 90.49(8) 2_576 2_666 ? N7 Mn1 N6 89.51(8) . 2_666 ? N1 Mn1 N6 86.50(8) 2_576 2_666 ? N1 Mn1 N6 93.50(8) . 2_666 ? N7 Mn1 N6 89.51(8) 2_576 1_465 ? N7 Mn1 N6 90.49(8) . 1_465 ? N1 Mn1 N6 93.50(8) 2_576 1_465 ? N1 Mn1 N6 86.50(8) . 1_465 ? N6 Mn1 N6 180.00 2_666 1_465 ? C1 N1 C2 116.6(3) . . ? C1 N1 Mn1 121.7(2) . . ? C2 N1 Mn1 121.45(19) . . ? C6 N2 N3 110.1(3) . . ? C7 N3 N2 114.2(3) . . ? C14 N4 N5 114.2(2) . . ? C21 N5 N4 113.4(2) . . ? C25 N6 C26 116.4(2) . . ? C25 N6 Mn1 119.41(18) . 1_645 ? C26 N6 Mn1 123.96(18) . 1_645 ? N1 C1 C5 124.5(3) . . ? N1 C1 H1A 117.7 . . ? C5 C1 H1A 117.7 . . ? N1 C2 C3 123.7(3) . . ? N1 C2 H2A 118.1 . . ? C3 C2 H2A 118.1 . . ? C2 C3 C4 118.6(3) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C4 C5 C1 117.3(3) . . ? C4 C5 C6 124.5(3) . . ? C1 C5 C6 118.1(3) . . ? N2 C6 C5 124.1(3) . . ? N2 C6 H6A 117.9 . . ? C5 C6 H6A 117.9 . . ? N3 C7 C8 118.1(3) . . ? N3 C7 C14 122.3(3) . . ? C8 C7 C14 119.5(2) . . ? C9 C8 C13 118.3(3) . . ? C9 C8 C7 120.2(3) . . ? C13 C8 C7 121.6(3) . . ? C10 C9 C8 120.0(3) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 120.3(3) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C12 C13 C8 121.1(3) . . ? C12 C13 H13A 119.5 . . ? C8 C13 H13A 119.5 . . ? N4 C14 C15 117.9(3) . . ? N4 C14 C7 124.0(2) . . ? C15 C14 C7 118.1(2) . . ? C20 C15 C16 117.7(3) . . ? C20 C15 C14 121.3(2) . . ? C16 C15 C14 120.9(3) . . ? C17 C16 C15 121.3(3) . . ? C17 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C19 C18 118.3(3) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? C15 C20 C19 121.7(3) . . ? C15 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? N5 C21 C22 120.0(3) . . ? N5 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C23 C22 C26 118.2(3) . . ? C23 C22 C21 120.6(2) . . ? C26 C22 C21 121.2(3) . . ? C24 C23 C22 119.0(3) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C23 C24 C25 119.0(3) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? N6 C25 C24 123.6(3) . . ? N6 C25 H25A 118.2 . . ? C24 C25 H25A 118.2 . . ? N6 C26 C22 123.7(3) . . ? N6 C26 H26A 118.2 . . ? C22 C26 H26A 118.2 . . ? C27 N7 Mn1 151.0(2) . . ? N7 C27 S1 178.1(3) . . ? C28 O1 H1B 109.5 . . ? O1 C28 C29 124.9(16) . . ? O1 C28 H28A 106.1 . . ? C29 C28 H28A 106.1 . . ? O1 C28 H28B 106.1 . . ? C29 C28 H28B 106.1 . . ? H28A C28 H28B 106.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28' O1' H1'A 109.5 . . ? O1' C28' C29' 122.3(16) . . ? O1' C28' H28C 106.8 . . ? C29' C28' H28C 106.8 . . ? O1' C28' H28D 106.8 . . ? C29' C28' H28D 106.8 . . ? H28C C28' H28D 106.6 . . ? C28' C29' H29D 109.5 . . ? C28' C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C28' C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.640 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.071 # Attachment '8.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 748797' #TrackingRef 'cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H40 N14 S2 Zn' _chemical_formula_sum 'C54 H40 N14 S2 Zn' _chemical_formula_weight 1014.49 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _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 19.9086(16) _cell_length_b 14.5963(12) _cell_length_c 17.3028(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.450(2) _cell_angle_gamma 90.00 _cell_volume 5026.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2338 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 23.16 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13188 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4668 _reflns_number_gt 3148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^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 4668 _refine_ls_number_parameters 321 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Zn1 Zn 0.0000 -0.05163(3) 0.2500 0.04281(14) Uani 1 2 d S . . N1 N -0.06396(10) -0.16000(13) 0.30147(11) 0.0437(5) Uani 1 1 d . . . N2 N -0.15988(11) -0.31021(15) 0.51447(12) 0.0533(6) Uani 1 1 d . . . N3 N -0.17945(11) -0.31105(14) 0.59181(12) 0.0499(6) Uani 1 1 d . . . N4 N -0.03233(11) -0.40400(14) 0.59893(13) 0.0517(6) Uani 1 1 d . . . N5 N -0.02133(11) -0.31328(14) 0.62556(13) 0.0551(6) Uani 1 1 d . . . N6 N 0.06107(10) -0.05648(13) 0.69974(11) 0.0427(5) Uani 1 1 d . . . C1 C -0.08208(12) -0.16370(16) 0.37539(14) 0.0443(6) Uani 1 1 d . . . H1A H -0.0680 -0.1168 0.4084 0.053 Uiso 1 1 calc R . . C2 C -0.08540(13) -0.22762(17) 0.25485(15) 0.0525(7) Uani 1 1 d . . . H2A H -0.0737 -0.2258 0.2032 0.063 Uiso 1 1 calc R . . C3 C -0.12382(15) -0.29956(19) 0.27949(16) 0.0629(8) Uani 1 1 d . . . H3A H -0.1372 -0.3457 0.2453 0.076 Uiso 1 1 calc R . . C4 C -0.14218(14) -0.30228(18) 0.35525(16) 0.0580(7) Uani 1 1 d . . . H4A H -0.1689 -0.3498 0.3729 0.070 Uiso 1 1 calc R . . C5 C -0.12067(12) -0.23358(16) 0.40551(14) 0.0438(6) Uani 1 1 d . . . C6 C -0.13817(13) -0.23636(18) 0.48744(15) 0.0494(7) Uani 1 1 d . . . H6A H -0.1333 -0.1847 0.5185 0.059 Uiso 1 1 calc R . . C7 C -0.14921(12) -0.37127(16) 0.63344(14) 0.0403(6) Uani 1 1 d . . . C8 C -0.17197(12) -0.39026(16) 0.71220(14) 0.0412(6) Uani 1 1 d . . . C9 C -0.23629(13) -0.36643(18) 0.73420(15) 0.0524(7) Uani 1 1 d . . . H9A H -0.2644 -0.3341 0.7002 0.063 Uiso 1 1 calc R . . C10 C -0.25858(15) -0.3906(2) 0.80608(17) 0.0656(9) Uani 1 1 d . . . H10A H -0.3017 -0.3742 0.8204 0.079 Uiso 1 1 calc R . . C11 C -0.21796(19) -0.4384(2) 0.85681(17) 0.0691(9) Uani 1 1 d . . . H11A H -0.2336 -0.4552 0.9050 0.083 Uiso 1 1 calc R . . C12 C -0.15429(18) -0.46142(19) 0.83628(17) 0.0659(8) Uani 1 1 d . . . H12A H -0.1263 -0.4927 0.8711 0.079 Uiso 1 1 calc R . . C13 C -0.13132(14) -0.43844(17) 0.76437(15) 0.0518(7) Uani 1 1 d . . . H13A H -0.0882 -0.4554 0.7506 0.062 Uiso 1 1 calc R . . C14 C -0.09358(13) -0.42975(16) 0.60382(14) 0.0425(6) Uani 1 1 d . . . C15 C -0.10999(13) -0.52636(16) 0.58331(14) 0.0428(6) Uani 1 1 d . . . C16 C -0.17602(13) -0.55313(18) 0.57089(15) 0.0522(7) Uani 1 1 d . . . H16A H -0.2102 -0.5100 0.5739 0.063 Uiso 1 1 calc R . . C17 C -0.19175(15) -0.6438(2) 0.55391(16) 0.0601(8) Uani 1 1 d . . . H17A H -0.2362 -0.6609 0.5444 0.072 Uiso 1 1 calc R . . C18 C -0.14179(17) -0.70775(19) 0.55128(16) 0.0630(8) Uani 1 1 d . . . H18A H -0.1523 -0.7688 0.5415 0.076 Uiso 1 1 calc R . . C19 C -0.07627(16) -0.68211(19) 0.56296(15) 0.0590(8) Uani 1 1 d . . . H19A H -0.0423 -0.7256 0.5599 0.071 Uiso 1 1 calc R . . C20 C -0.06013(14) -0.59207(18) 0.57921(15) 0.0537(7) Uani 1 1 d . . . H20A H -0.0154 -0.5755 0.5875 0.064 Uiso 1 1 calc R . . C21 C 0.04068(13) -0.29376(16) 0.61983(14) 0.0440(6) Uani 1 1 d . . . H21A H 0.0685 -0.3364 0.5966 0.053 Uiso 1 1 calc R . . C22 C 0.07072(12) -0.20774(16) 0.64777(14) 0.0426(6) Uani 1 1 d . . . C23 C 0.03387(12) -0.13177(17) 0.66811(14) 0.0435(6) Uani 1 1 d . . . H23A H -0.0124 -0.1330 0.6593 0.052 Uiso 1 1 calc R . . C24 C 0.12782(13) -0.05458(18) 0.70992(15) 0.0512(7) Uani 1 1 d . . . H24A H 0.1475 -0.0027 0.7321 0.061 Uiso 1 1 calc R . . C25 C 0.16858(13) -0.12567(19) 0.68915(16) 0.0564(7) Uani 1 1 d . . . H25A H 0.2149 -0.1216 0.6964 0.068 Uiso 1 1 calc R . . C26 C 0.13980(13) -0.20286(18) 0.65757(15) 0.0497(7) Uani 1 1 d . . . H26A H 0.1666 -0.2517 0.6428 0.060 Uiso 1 1 calc R . . S1 S 0.12709(5) -0.03091(6) 0.49231(5) 0.0780(3) Uani 1 1 d . . . C27 C 0.08786(13) -0.04299(16) 0.40914(15) 0.0446(6) Uani 1 1 d . . . N7 N 0.06123(11) -0.05272(14) 0.34960(12) 0.0522(6) 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 Zn1 0.0499(3) 0.0399(3) 0.0387(2) 0.000 0.00197(19) 0.000 N1 0.0569(14) 0.0373(12) 0.0370(12) -0.0037(9) 0.0046(10) -0.0036(10) N2 0.0718(16) 0.0480(14) 0.0405(13) 0.0091(11) 0.0061(11) 0.0028(12) N3 0.0620(14) 0.0432(13) 0.0450(13) 0.0069(10) 0.0105(11) 0.0013(11) N4 0.0508(14) 0.0404(13) 0.0644(16) -0.0113(11) 0.0109(11) -0.0061(11) N5 0.0501(14) 0.0446(14) 0.0712(16) -0.0139(11) 0.0123(12) -0.0070(11) N6 0.0398(12) 0.0401(12) 0.0481(13) -0.0024(10) 0.0019(10) -0.0040(10) C1 0.0592(17) 0.0362(14) 0.0377(15) -0.0024(11) 0.0049(12) 0.0004(12) C2 0.0724(19) 0.0454(16) 0.0398(16) -0.0034(12) 0.0070(14) -0.0033(14) C3 0.091(2) 0.0474(17) 0.0510(18) -0.0088(14) 0.0073(16) -0.0198(16) C4 0.078(2) 0.0417(16) 0.0543(18) 0.0032(13) 0.0064(15) -0.0113(14) C5 0.0535(16) 0.0348(14) 0.0431(15) 0.0057(12) 0.0049(12) 0.0029(12) C6 0.0615(18) 0.0422(16) 0.0449(16) 0.0044(12) 0.0078(13) 0.0035(13) C7 0.0431(15) 0.0336(14) 0.0442(15) 0.0008(12) 0.0039(12) -0.0042(12) C8 0.0474(15) 0.0358(14) 0.0405(15) 0.0003(11) 0.0036(12) -0.0079(12) C9 0.0461(16) 0.0641(19) 0.0469(17) -0.0035(13) 0.0013(13) -0.0081(14) C10 0.0549(18) 0.090(2) 0.0524(19) -0.0128(17) 0.0143(16) -0.0240(17) C11 0.100(3) 0.068(2) 0.0404(17) 0.0017(15) 0.0078(18) -0.037(2) C12 0.098(3) 0.0504(19) 0.0495(18) 0.0057(14) -0.0060(18) -0.0060(18) C13 0.0663(18) 0.0440(15) 0.0449(16) 0.0031(13) 0.0026(14) 0.0032(14) C14 0.0483(16) 0.0395(15) 0.0399(14) 0.0017(11) 0.0039(12) -0.0044(12) C15 0.0525(17) 0.0376(14) 0.0386(15) -0.0006(11) 0.0051(12) -0.0030(13) C16 0.0553(18) 0.0492(17) 0.0520(17) -0.0036(13) -0.0001(13) -0.0004(14) C17 0.069(2) 0.0544(19) 0.0565(18) -0.0050(14) 0.0003(15) -0.0205(17) C18 0.095(3) 0.0407(17) 0.0533(18) -0.0062(13) 0.0037(17) -0.0119(18) C19 0.081(2) 0.0444(17) 0.0520(18) -0.0008(13) 0.0042(16) 0.0100(16) C20 0.0581(18) 0.0485(17) 0.0545(18) -0.0039(13) 0.0050(14) 0.0014(14) C21 0.0477(16) 0.0401(15) 0.0442(15) -0.0024(12) 0.0046(12) 0.0012(13) C22 0.0443(15) 0.0390(15) 0.0448(15) 0.0016(11) 0.0051(12) 0.0007(12) C23 0.0366(14) 0.0459(16) 0.0481(15) -0.0009(12) 0.0021(11) -0.0025(12) C24 0.0487(17) 0.0474(16) 0.0575(17) -0.0067(13) -0.0011(13) -0.0091(14) C25 0.0379(15) 0.0580(18) 0.073(2) -0.0032(15) -0.0015(14) -0.0015(14) C26 0.0420(16) 0.0464(16) 0.0609(18) 0.0012(13) 0.0052(13) 0.0066(13) S1 0.1062(7) 0.0767(6) 0.0500(5) -0.0143(4) -0.0191(5) 0.0169(5) C27 0.0529(16) 0.0346(15) 0.0468(16) -0.0011(12) 0.0118(14) 0.0063(12) N7 0.0588(14) 0.0579(14) 0.0397(13) -0.0039(11) 0.0003(11) 0.0048(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 Zn1 N7 2.086(2) . ? Zn1 N7 2.086(2) 2 ? Zn1 N6 2.1859(19) 6 ? Zn1 N6 2.1859(19) 5_556 ? Zn1 N1 2.2303(19) . ? Zn1 N1 2.2303(19) 2 ? N1 C2 1.338(3) . ? N1 C1 1.339(3) . ? N2 C6 1.256(3) . ? N2 N3 1.403(3) . ? N3 C7 1.277(3) . ? N4 C14 1.281(3) . ? N4 N5 1.417(3) . ? N5 C21 1.273(3) . ? N6 C23 1.336(3) . ? N6 C24 1.336(3) . ? N6 Zn1 2.1859(19) 5_556 ? C1 C5 1.386(3) . ? C1 H1A 0.9300 . ? C2 C3 1.373(3) . ? C2 H2A 0.9300 . ? C3 C4 1.370(4) . ? C3 H3A 0.9300 . ? C4 C5 1.388(3) . ? C4 H4A 0.9300 . ? C5 C6 1.469(3) . ? C6 H6A 0.9300 . ? C7 C8 1.473(3) . ? C7 C14 1.499(3) . ? C8 C13 1.388(3) . ? C8 C9 1.389(3) . ? C9 C10 1.377(4) . ? C9 H9A 0.9300 . ? C10 C11 1.370(4) . ? C10 H10A 0.9300 . ? C11 C12 1.367(4) . ? C11 H11A 0.9300 . ? C12 C13 1.378(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.488(3) . ? C15 C16 1.383(3) . ? C15 C20 1.383(3) . ? C16 C17 1.390(3) . ? C16 H16A 0.9300 . ? C17 C18 1.365(4) . ? C17 H17A 0.9300 . ? C18 C19 1.367(4) . ? C18 H18A 0.9300 . ? C19 C20 1.380(4) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.467(3) . ? C21 H21A 0.9300 . ? C22 C23 1.380(3) . ? C22 C26 1.383(3) . ? C23 H23A 0.9300 . ? C24 C25 1.371(3) . ? C24 H24A 0.9300 . ? C25 C26 1.371(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? S1 C27 1.629(3) . ? C27 N7 1.155(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 N7 Zn1 N7 179.12(12) . 2 ? N7 Zn1 N6 90.85(8) . 6 ? N7 Zn1 N6 89.78(8) 2 6 ? N7 Zn1 N6 89.78(8) . 5_556 ? N7 Zn1 N6 90.85(8) 2 5_556 ? N6 Zn1 N6 87.58(10) 6 5_556 ? N7 Zn1 N1 89.56(8) . . ? N7 Zn1 N1 89.82(8) 2 . ? N6 Zn1 N1 178.88(7) 6 . ? N6 Zn1 N1 91.39(7) 5_556 . ? N7 Zn1 N1 89.82(8) . 2 ? N7 Zn1 N1 89.56(8) 2 2 ? N6 Zn1 N1 91.39(7) 6 2 ? N6 Zn1 N1 178.88(7) 5_556 2 ? N1 Zn1 N1 89.65(10) . 2 ? C2 N1 C1 117.2(2) . . ? C2 N1 Zn1 117.33(17) . . ? C1 N1 Zn1 125.48(16) . . ? C6 N2 N3 118.0(2) . . ? C7 N3 N2 113.9(2) . . ? C14 N4 N5 113.1(2) . . ? C21 N5 N4 109.0(2) . . ? C23 N6 C24 117.5(2) . . ? C23 N6 Zn1 122.21(16) . 5_556 ? C24 N6 Zn1 119.59(16) . 5_556 ? N1 C1 C5 123.6(2) . . ? N1 C1 H1A 118.2 . . ? C5 C1 H1A 118.2 . . ? N1 C2 C3 123.3(2) . . ? N1 C2 H2A 118.4 . . ? C3 C2 H2A 118.4 . . ? C4 C3 C2 118.9(2) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 119.5(2) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C1 C5 C4 117.5(2) . . ? C1 C5 C6 122.0(2) . . ? C4 C5 C6 120.5(2) . . ? N2 C6 C5 118.4(2) . . ? N2 C6 H6A 120.8 . . ? C5 C6 H6A 120.8 . . ? N3 C7 C8 120.0(2) . . ? N3 C7 C14 122.7(2) . . ? C8 C7 C14 117.2(2) . . ? C13 C8 C9 118.3(2) . . ? C13 C8 C7 120.6(2) . . ? C9 C8 C7 120.9(2) . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 120.7(3) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C12 C11 C10 119.7(3) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C12 C13 C8 120.6(3) . . ? C12 C13 H13A 119.7 . . ? C8 C13 H13A 119.7 . . ? N4 C14 C15 117.8(2) . . ? N4 C14 C7 124.6(2) . . ? C15 C14 C7 117.5(2) . . ? C16 C15 C20 118.5(2) . . ? C16 C15 C14 120.5(2) . . ? C20 C15 C14 121.0(2) . . ? C15 C16 C17 120.7(3) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C18 C17 C16 119.8(3) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 120.1(3) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C18 C19 C20 120.5(3) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C15 120.5(3) . . ? C19 C20 H20A 119.8 . . ? C15 C20 H20A 119.8 . . ? N5 C21 C22 123.6(2) . . ? N5 C21 H21A 118.2 . . ? C22 C21 H21A 118.2 . . ? C23 C22 C26 117.4(2) . . ? C23 C22 C21 123.8(2) . . ? C26 C22 C21 118.7(2) . . ? N6 C23 C22 123.6(2) . . ? N6 C23 H23A 118.2 . . ? C22 C23 H23A 118.2 . . ? N6 C24 C25 122.9(2) . . ? N6 C24 H24A 118.6 . . ? C25 C24 H24A 118.6 . . ? C24 C25 C26 118.8(2) . . ? C24 C25 H25A 120.6 . . ? C26 C25 H25A 120.6 . . ? C25 C26 C22 119.7(2) . . ? C25 C26 H26A 120.2 . . ? C22 C26 H26A 120.2 . . ? N7 C27 S1 178.5(2) . . ? C27 N7 Zn1 168.9(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.380 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.047