# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name 'Kumar Biradha' _publ_contact_author_name 'Kumar Biradha' _publ_contact_author_email 'kbiradha@yahoo.com ' data_2 _database_code_depnum_ccdc_archive 'CCDC 891754' #TrackingRef '- kbss.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H34 N6 O2' _chemical_formula_weight 570.68 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.398(2) _cell_length_b 12.489(3) _cell_length_c 24.239(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.067(7) _cell_angle_gamma 90.00 _cell_volume 3099.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 33705 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.988 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD APEX 2' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33705 _diffrn_reflns_av_R_equivalents 0.1916 _diffrn_reflns_av_sigmaI/netI 0.1709 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5314 _reflns_number_gt 1740 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1997P)^2^+0.0634P] 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 5314 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1691 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.2358 _refine_ls_wR_factor_gt 0.1898 _refine_ls_goodness_of_fit_ref 0.547 _refine_ls_restrained_S_all 0.547 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.004 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 O1W O -0.1632(3) 0.38152(19) -0.12973(10) 0.1163(13) Uani 1 1 d . . . O2W O 0.0291(3) 0.6261(2) 0.21970(12) 0.1307(14) Uani 1 1 d . . . N22A N 0.4317(3) 0.3226(2) 0.22582(12) 0.1020(13) Uani 1 1 d . . . H22A H 0.4426 0.2622 0.2431 0.122 Uiso 1 1 calc R . . N22B N 0.0949(3) 0.4360(3) 0.28642(12) 0.1055(13) Uani 1 1 d . . . N21A N 0.3311(3) 0.4562(2) 0.17477(12) 0.1028(13) Uani 1 1 d . . . N11A N -0.0765(5) 0.3532(4) -0.01565(16) 0.1371(16) Uani 1 1 d . . . C16A C 0.0669(3) 0.3459(3) 0.16221(14) 0.0978(13) Uani 1 1 d . . . H16A H 0.0638 0.4192 0.1763 0.117 Uiso 1 1 calc R . . C21A C 0.3175(3) 0.3612(3) 0.19680(14) 0.0959(13) Uani 1 1 d . . . N21B N 0.2156(3) 0.3128(2) 0.33795(13) 0.1062(13) Uani 1 1 d . . . H21B H 0.2565 0.2537 0.3467 0.127 Uiso 1 1 calc R . . C21B C 0.1466(3) 0.3392(3) 0.28669(14) 0.0980(13) Uani 1 1 d . . . C16B C -0.0029(3) 0.2695(3) 0.20023(14) 0.0988(14) Uani 1 1 d . . . H16B H -0.0679 0.3074 0.2176 0.119 Uiso 1 1 calc R . . C17B C 0.1310(3) 0.2616(3) 0.23964(14) 0.0982(14) Uani 1 1 d . . . H17B H 0.1537 0.1882 0.2519 0.118 Uiso 1 1 calc R . . C13A C 0.0192(3) 0.3477(3) 0.09955(14) 0.0967(13) Uani 1 1 d . . . C22A C 0.5275(4) 0.3983(3) 0.22237(15) 0.1031(14) Uani 1 1 d . . . C23A C 0.4634(4) 0.4806(3) 0.19100(15) 0.1019(14) Uani 1 1 d . . . C22B C 0.2077(4) 0.3981(3) 0.37330(16) 0.1097(14) Uani 1 1 d . . . C27A C 0.6588(4) 0.3985(4) 0.2444(2) 0.1260(16) Uani 1 1 d . . . H27A H 0.6987 0.3424 0.2662 0.151 Uiso 1 1 calc R . . C17A C 0.1954(3) 0.2971(3) 0.18837(13) 0.0972(13) Uani 1 1 d . . . H17A H 0.2094 0.2329 0.1669 0.117 Uiso 1 1 calc R . . C12A C 0.0662(4) 0.2837(4) 0.06270(17) 0.1292(17) Uani 1 1 d . . . H12A H 0.1327 0.2355 0.0758 0.155 Uiso 1 1 calc R . . C13B C -0.0573(4) 0.1690(3) 0.17057(14) 0.1041(14) Uani 1 1 d . . . C14B C 0.0145(4) 0.0769(3) 0.16629(17) 0.1166(15) Uani 1 1 d . . . H14B H 0.1017 0.0735 0.1834 0.140 Uiso 1 1 calc R . . C23B C 0.1312(4) 0.4747(3) 0.34042(15) 0.1035(14) Uani 1 1 d . . . C24B C 0.1031(5) 0.5709(3) 0.36389(18) 0.1245(16) Uani 1 1 d . . . H24B H 0.0534 0.6232 0.3427 0.149 Uiso 1 1 calc R . . C27B C 0.2578(5) 0.4176(4) 0.42979(18) 0.1336(17) Uani 1 1 d . . . H27B H 0.3089 0.3668 0.4515 0.160 Uiso 1 1 calc R . . C24A C 0.5345(5) 0.5702(4) 0.1788(2) 0.1305(16) Uani 1 1 d . . . H24A H 0.4945 0.6266 0.1573 0.157 Uiso 1 1 calc R . . N11B N -0.1648(6) -0.0077(4) 0.1090(2) 0.1640(18) Uani 1 1 d . . . C12B C -0.1855(4) 0.1678(4) 0.14358(19) 0.1322(17) Uani 1 1 d . . . H12B H -0.2389 0.2267 0.1461 0.159 Uiso 1 1 calc R . . C25B C 0.1519(6) 0.5863(4) 0.4201(2) 0.1379(18) Uani 1 1 d . . . H25B H 0.1311 0.6493 0.4370 0.165 Uiso 1 1 calc R . . C14A C -0.0766(5) 0.4169(4) 0.07654(18) 0.1320(17) Uani 1 1 d . . . H14A H -0.1117 0.4647 0.0993 0.158 Uiso 1 1 calc R . . C15B C -0.0431(6) -0.0089(4) 0.1369(2) 0.1360(17) Uani 1 1 d . . . H15B H 0.0054 -0.0713 0.1364 0.163 Uiso 1 1 calc R . . C26A C 0.7269(5) 0.4869(5) 0.2322(2) 0.1358(17) Uani 1 1 d . . . H26A H 0.8162 0.4902 0.2458 0.163 Uiso 1 1 calc R . . C26B C 0.2299(6) 0.5125(4) 0.4521(2) 0.1455(19) Uani 1 1 d . . . H26B H 0.2638 0.5278 0.4893 0.175 Uiso 1 1 calc R . . C15A C -0.1213(5) 0.4163(4) 0.0198(3) 0.1474(19) Uani 1 1 d . . . H15A H -0.1877 0.4639 0.0056 0.177 Uiso 1 1 calc R . . C11A C 0.0178(6) 0.2884(5) 0.0067(2) 0.1480(19) Uani 1 1 d . . . H11A H 0.0538 0.2432 -0.0170 0.178 Uiso 1 1 calc R . . C25A C 0.6688(5) 0.5709(4) 0.2006(2) 0.1427(19) Uani 1 1 d . . . H25A H 0.7192 0.6291 0.1935 0.171 Uiso 1 1 calc R . . C11B C -0.2346(6) 0.0798(6) 0.1130(2) 0.156(2) Uani 1 1 d . . . H11B H -0.3206 0.0817 0.0943 0.187 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 O1W 0.144(2) 0.1047(19) 0.0986(18) 0.0004(12) 0.0170(14) -0.0068(14) O2W 0.154(3) 0.107(2) 0.135(2) -0.0077(14) 0.0358(17) -0.0053(16) N22A 0.099(2) 0.105(2) 0.103(2) 0.0063(15) 0.0198(16) 0.0002(17) N22B 0.117(2) 0.101(2) 0.103(2) 0.0025(16) 0.0298(16) -0.0027(17) N21A 0.106(2) 0.103(2) 0.099(2) 0.0093(15) 0.0185(15) -0.0009(16) N11A 0.143(3) 0.160(4) 0.103(3) 0.009(2) 0.008(2) -0.017(3) C16A 0.096(2) 0.095(2) 0.101(2) 0.0020(17) 0.0143(18) -0.0056(18) C21A 0.091(3) 0.105(3) 0.092(2) -0.0044(18) 0.0176(18) 0.005(2) N21B 0.117(2) 0.097(2) 0.104(2) 0.0004(16) 0.0146(17) 0.0032(16) C21B 0.095(2) 0.107(3) 0.091(2) 0.0087(19) 0.0157(18) -0.005(2) C16B 0.095(2) 0.101(3) 0.102(2) -0.0025(18) 0.0217(18) -0.0018(18) C17B 0.106(3) 0.099(2) 0.094(2) 0.0032(17) 0.0290(19) 0.0002(18) C13A 0.101(2) 0.102(2) 0.087(2) 0.0043(18) 0.0160(18) -0.0054(19) C22A 0.094(3) 0.112(3) 0.104(3) -0.012(2) 0.0190(19) -0.004(2) C23A 0.097(3) 0.109(3) 0.101(2) -0.002(2) 0.0230(19) 0.001(2) C22B 0.126(3) 0.107(3) 0.095(3) -0.005(2) 0.017(2) -0.005(2) C27A 0.105(3) 0.125(3) 0.146(4) -0.007(3) 0.016(3) -0.002(2) C17A 0.099(3) 0.106(2) 0.086(2) 0.0031(16) 0.0176(17) -0.0078(18) C12A 0.131(3) 0.161(4) 0.092(3) -0.004(2) 0.010(2) 0.013(3) C13B 0.107(3) 0.118(3) 0.092(2) 0.003(2) 0.028(2) -0.012(2) C14B 0.118(3) 0.109(3) 0.125(3) -0.007(2) 0.029(2) -0.018(2) C23B 0.114(3) 0.107(3) 0.091(2) -0.005(2) 0.0221(19) -0.007(2) C24B 0.163(4) 0.107(3) 0.114(3) -0.001(2) 0.052(3) 0.001(2) C27B 0.150(4) 0.139(4) 0.108(3) 0.005(3) 0.015(3) 0.002(3) C24A 0.126(4) 0.122(3) 0.148(4) 0.008(2) 0.036(3) -0.017(3) N11B 0.174(5) 0.163(4) 0.152(4) -0.034(3) 0.021(3) -0.030(4) C12B 0.108(3) 0.151(4) 0.133(3) -0.006(3) 0.009(3) -0.022(3) C25B 0.183(5) 0.123(4) 0.117(4) -0.023(3) 0.054(3) -0.014(3) C14A 0.139(4) 0.142(4) 0.103(3) 0.007(2) -0.011(2) 0.019(3) C15B 0.138(4) 0.135(4) 0.134(4) -0.016(3) 0.022(3) -0.019(3) C26A 0.108(3) 0.142(4) 0.156(4) -0.006(3) 0.020(3) -0.010(3) C26B 0.206(5) 0.128(4) 0.105(3) -0.013(3) 0.034(3) -0.001(4) C15A 0.145(4) 0.145(4) 0.141(4) 0.027(3) -0.007(3) 0.012(3) C11A 0.145(4) 0.196(5) 0.100(3) 0.003(3) 0.015(3) 0.004(4) C25A 0.118(4) 0.138(4) 0.176(5) -0.017(3) 0.039(3) -0.028(3) C11B 0.120(4) 0.176(5) 0.160(4) -0.020(4) -0.008(3) -0.017(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N22A C21A 1.359(4) . ? N22A C22A 1.387(5) . ? N22B C21B 1.324(4) . ? N22B C23B 1.384(5) . ? N21A C21A 1.318(4) . ? N21A C23A 1.396(5) . ? N11A C11A 1.313(6) . ? N11A C15A 1.311(6) . ? C16A C13A 1.513(5) . ? C16A C17A 1.505(5) . ? C16A C16B 1.587(5) . ? C21A C17A 1.485(5) . ? N21B C21B 1.362(4) . ? N21B C22B 1.378(4) . ? C21B C17B 1.484(5) . ? C16B C13B 1.506(5) . ? C16B C17B 1.548(5) . ? C17B C17A 1.575(5) . ? C13A C12A 1.352(5) . ? C13A C14A 1.363(5) . ? C22A C27A 1.377(5) . ? C22A C23A 1.378(5) . ? C23A C24A 1.401(5) . ? C22B C23B 1.401(5) . ? C22B C27B 1.399(6) . ? C27A C26A 1.372(6) . ? C12A C11A 1.363(6) . ? C13B C12B 1.379(5) . ? C13B C14B 1.385(5) . ? C14B C15B 1.366(6) . ? C23B C24B 1.383(5) . ? C24B C25B 1.381(6) . ? C27B C26B 1.355(6) . ? C24A C25A 1.404(7) . ? N11B C11B 1.324(7) . ? N11B C15B 1.326(6) . ? C12B C11B 1.373(7) . ? C25B C26B 1.374(7) . ? C14A C15A 1.373(7) . ? C26A C25A 1.375(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 C21A N22A C22A 107.3(3) . . ? C21B N22B C23B 105.7(3) . . ? C21A N21A C23A 104.6(3) . . ? C11A N11A C15A 115.1(4) . . ? C13A C16A C17A 122.7(3) . . ? C13A C16A C16B 119.3(3) . . ? C17A C16A C16B 88.5(2) . . ? N21A C21A N22A 112.5(3) . . ? N21A C21A C17A 125.4(3) . . ? N22A C21A C17A 121.9(3) . . ? C21B N21B C22B 107.6(3) . . ? N22B C21B N21B 112.0(3) . . ? N22B C21B C17B 127.1(3) . . ? N21B C21B C17B 120.9(3) . . ? C13B C16B C17B 117.6(3) . . ? C13B C16B C16A 113.3(3) . . ? C17B C16B C16A 86.8(2) . . ? C21B C17B C16B 113.5(3) . . ? C21B C17B C17A 114.7(3) . . ? C16B C17B C17A 87.5(2) . . ? C12A C13A C14A 115.3(4) . . ? C12A C13A C16A 124.1(3) . . ? C14A C13A C16A 120.5(4) . . ? C27A C22A C23A 124.3(4) . . ? C27A C22A N22A 130.6(4) . . ? C23A C22A N22A 105.0(3) . . ? C22A C23A N21A 110.5(3) . . ? C22A C23A C24A 119.3(4) . . ? N21A C23A C24A 130.1(4) . . ? N21B C22B C23B 105.3(3) . . ? N21B C22B C27B 133.7(4) . . ? C23B C22B C27B 121.0(4) . . ? C26A C27A C22A 115.6(4) . . ? C21A C17A C16A 121.0(3) . . ? C21A C17A C17B 121.0(3) . . ? C16A C17A C17B 88.7(3) . . ? C13A C12A C11A 121.2(5) . . ? C12B C13B C14B 116.4(4) . . ? C12B C13B C16B 119.1(4) . . ? C14B C13B C16B 124.4(3) . . ? C15B C14B C13B 119.8(4) . . ? N22B C23B C24B 130.5(4) . . ? N22B C23B C22B 109.5(3) . . ? C24B C23B C22B 120.0(4) . . ? C23B C24B C25B 117.3(4) . . ? C26B C27B C22B 118.3(4) . . ? C25A C24A C23A 116.9(4) . . ? C11B N11B C15B 117.2(5) . . ? C11B C12B C13B 120.1(5) . . ? C26B C25B C24B 122.8(4) . . ? C13A C14A C15A 120.1(5) . . ? N11B C15B C14B 123.3(5) . . ? C27A C26A C25A 122.8(4) . . ? C27B C26B C25B 120.5(4) . . ? N11A C15A C14A 124.3(5) . . ? N11A C11A C12A 123.8(5) . . ? C26A C25A C24A 121.1(5) . . ? N11B C11B C12B 122.9(5) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.043 _refine_diff_density_min -0.034 _refine_diff_density_rms 0.010 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 389 124 ' ' 2 0.500 0.498 1.000 389 124 ' ' _platon_squeeze_details ; ; data_3 _database_code_depnum_ccdc_archive 'CCDC 891755' #TrackingRef '- kbss.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H15 Ag N4 O4' _chemical_formula_weight 423.18 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 P21/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 7.750(2) _cell_length_b 19.835(5) _cell_length_c 10.502(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.438(9) _cell_angle_gamma 90.00 _cell_volume 1592.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17927 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.765 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 1.294 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD apex 2' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17927 _diffrn_reflns_av_R_equivalents 0.2339 _diffrn_reflns_av_sigmaI/netI 0.1548 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2717 _reflns_number_gt 1137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^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 2717 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2042 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.1902 _refine_ls_wR_factor_gt 0.1487 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.836 _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 0.38072(13) 0.71655(4) 0.14544(9) 0.0681(4) Uani 1 1 d . . . N11 N 0.1165(11) 0.5788(4) -0.1453(8) 0.046(2) Uani 1 1 d . . . H11 H 0.0931 0.5397 -0.1792 0.055 Uiso 1 1 calc R . . N12 N 0.2307(11) 0.6570(4) -0.0044(8) 0.046(2) Uani 1 1 d . . . C11 C 0.2122(14) 0.5909(4) -0.0296(10) 0.042(3) Uani 1 1 d . . . C12 C 0.0627(14) 0.6388(5) -0.2001(10) 0.043(3) Uani 1 1 d . . . C13 C 0.1388(13) 0.6884(5) -0.1144(9) 0.040(3) Uani 1 1 d . . . C14 C 0.1151(15) 0.7579(5) -0.1409(12) 0.056(3) Uani 1 1 d . . . H14 H 0.1607 0.7910 -0.0823 0.067 Uiso 1 1 calc R . . C15 C 0.0160(17) 0.7737(7) -0.2643(15) 0.084(4) Uani 1 1 d . . . H15 H -0.0008 0.8184 -0.2899 0.101 Uiso 1 1 calc R . . C16 C -0.0532(17) 0.7235(5) -0.3440(11) 0.069(4) Uani 1 1 d . . . H16 H -0.1165 0.7358 -0.4236 0.083 Uiso 1 1 calc R . . C17 C -0.0372(15) 0.6572(7) -0.3165(12) 0.067(4) Uani 1 1 d . . . H17 H -0.0914 0.6249 -0.3738 0.080 Uiso 1 1 calc R . . N21 N 0.4921(11) 0.3055(4) 0.2571(8) 0.043(2) Uani 1 1 d . . . C21 C 0.5199(16) 0.3699(6) 0.2997(11) 0.068(4) Uani 1 1 d . . . H21 H 0.5902 0.3760 0.3795 0.082 Uiso 1 1 calc R . . C22 C 0.4548(16) 0.4251(5) 0.2366(11) 0.062(3) Uani 1 1 d . . . H22 H 0.4805 0.4675 0.2723 0.074 Uiso 1 1 calc R . . C23 C 0.3506(14) 0.4188(5) 0.1197(10) 0.047(3) Uani 1 1 d . . . C24 C 0.3210(16) 0.3525(5) 0.0686(11) 0.058(3) Uani 1 1 d . . . H24 H 0.2566 0.3450 -0.0130 0.070 Uiso 1 1 calc R . . C25 C 0.3924(16) 0.3003(5) 0.1457(12) 0.058(3) Uani 1 1 d . . . H25 H 0.3665 0.2569 0.1150 0.070 Uiso 1 1 calc R . . C26 C 0.2763(15) 0.4752(5) 0.0383(10) 0.051(3) Uani 1 1 d . . . H26 H 0.2087 0.4631 -0.0399 0.062 Uiso 1 1 calc R . . C27 C 0.2915(15) 0.5394(5) 0.0598(10) 0.051(3) Uani 1 1 d . . . H27 H 0.3572 0.5535 0.1374 0.061 Uiso 1 1 calc R . . N100 N 0.5990(19) 0.6140(6) 0.3472(15) 0.078(3) Uani 1 1 d . . . O101 O 0.6520(15) 0.6220(6) 0.2411(14) 0.120(4) Uani 1 1 d . . . O102 O 0.674(2) 0.5741(6) 0.4220(14) 0.159(6) Uani 1 1 d . . . O103 O 0.4632(14) 0.6433(5) 0.3643(9) 0.091(3) Uani 1 1 d . . . O1M O 1.0375(13) 0.4592(5) 0.7252(11) 0.103(4) Uani 1 1 d . . . C1M C 0.889(2) 0.4533(7) 0.6293(16) 0.109(5) Uani 1 1 d . . . H1M1 H 0.7870 0.4481 0.6692 0.163 Uiso 1 1 calc R . . H1M2 H 0.9016 0.4146 0.5767 0.163 Uiso 1 1 calc R . . H1M3 H 0.8776 0.4930 0.5766 0.163 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 0.0846(7) 0.0396(5) 0.0700(7) -0.0090(5) -0.0173(5) -0.0086(6) N11 0.063(5) 0.017(4) 0.052(5) 0.000(4) -0.005(4) 0.003(4) N12 0.052(6) 0.040(5) 0.041(5) -0.003(4) -0.003(4) 0.001(4) C11 0.052(7) 0.017(5) 0.053(7) 0.001(4) -0.005(6) 0.001(5) C12 0.049(7) 0.047(7) 0.033(6) -0.006(5) 0.005(5) -0.001(6) C13 0.040(6) 0.036(5) 0.045(7) 0.004(5) 0.008(6) 0.002(5) C14 0.055(7) 0.036(6) 0.076(8) 0.013(6) 0.008(6) 0.008(6) C15 0.077(9) 0.051(9) 0.121(12) 0.009(9) 0.007(9) 0.025(8) C16 0.106(10) 0.029(7) 0.061(8) 0.001(6) -0.021(7) -0.003(7) C17 0.050(7) 0.067(9) 0.077(9) -0.008(7) -0.011(7) 0.010(7) N21 0.057(6) 0.028(5) 0.040(5) 0.002(4) -0.007(4) 0.007(4) C21 0.062(8) 0.071(9) 0.062(8) -0.011(7) -0.020(7) 0.015(7) C22 0.097(10) 0.019(6) 0.061(8) 0.002(5) -0.010(7) 0.013(6) C23 0.058(8) 0.024(5) 0.059(8) 0.007(5) 0.008(6) -0.005(5) C24 0.091(9) 0.032(6) 0.045(7) 0.000(5) -0.009(6) -0.008(6) C25 0.076(8) 0.022(6) 0.067(8) -0.008(5) -0.014(6) -0.004(6) C26 0.074(8) 0.039(7) 0.039(7) -0.009(5) 0.002(6) 0.000(6) C27 0.067(8) 0.041(7) 0.042(7) -0.004(5) 0.001(6) -0.006(6) N100 0.081(9) 0.047(7) 0.104(11) -0.004(8) 0.010(9) 0.008(7) O101 0.100(9) 0.130(10) 0.136(11) -0.002(9) 0.034(9) 0.029(7) O102 0.207(14) 0.090(9) 0.160(12) 0.028(9) -0.030(10) 0.071(10) O103 0.096(7) 0.081(7) 0.102(8) 0.027(6) 0.028(6) 0.015(6) O1M 0.089(8) 0.074(7) 0.133(9) -0.044(6) -0.021(7) 0.019(5) C1M 0.136(15) 0.067(10) 0.118(14) 0.007(9) 0.004(13) 0.020(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 N12 2.150(8) . ? Ag1 N21 2.192(7) 2_655 ? N11 C11 1.338(11) . ? N11 C12 1.358(12) . ? N12 C11 1.340(11) . ? N12 C13 1.400(11) . ? C11 C27 1.453(14) . ? C12 C17 1.385(14) . ? C12 C13 1.397(13) . ? C13 C14 1.412(14) . ? C14 C15 1.428(17) . ? C15 C16 1.353(16) . ? C16 C17 1.349(15) . ? N21 C25 1.296(12) . ? N21 C21 1.358(13) . ? N21 Ag1 2.192(7) 2_645 ? C21 C22 1.335(14) . ? C22 C23 1.360(15) . ? C23 C24 1.423(13) . ? C23 C26 1.468(13) . ? C24 C25 1.374(14) . ? C26 C27 1.296(13) . ? N100 O102 1.197(15) . ? N100 O103 1.241(14) . ? N100 O101 1.260(14) . ? O1M C1M 1.403(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Ag1 N21 158.8(3) . 2_655 ? C11 N11 C12 108.2(8) . . ? C11 N12 C13 104.4(8) . . ? C11 N12 Ag1 135.2(7) . . ? C13 N12 Ag1 120.0(6) . . ? N11 C11 N12 112.4(8) . . ? N11 C11 C27 125.0(9) . . ? N12 C11 C27 122.7(9) . . ? C17 C12 N11 133.9(10) . . ? C17 C12 C13 119.9(10) . . ? N11 C12 C13 106.1(9) . . ? C12 C13 N12 108.8(9) . . ? C12 C13 C14 122.2(10) . . ? N12 C13 C14 129.0(9) . . ? C15 C14 C13 115.2(11) . . ? C16 C15 C14 120.0(11) . . ? C17 C16 C15 124.9(12) . . ? C16 C17 C12 117.6(11) . . ? C25 N21 C21 114.3(8) . . ? C25 N21 Ag1 120.9(6) . 2_645 ? C21 N21 Ag1 124.6(7) . 2_645 ? C22 C21 N21 125.5(11) . . ? C21 C22 C23 119.5(11) . . ? C22 C23 C24 117.5(9) . . ? C22 C23 C26 125.0(9) . . ? C24 C23 C26 117.4(9) . . ? C25 C24 C23 116.6(10) . . ? N21 C25 C24 126.5(9) . . ? C27 C26 C23 129.2(10) . . ? C26 C27 C11 124.1(10) . . ? O102 N100 O103 123.2(17) . . ? O102 N100 O101 118.0(16) . . ? O103 N100 O101 118.5(13) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.909 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.117 data_4 _database_code_depnum_ccdc_archive 'CCDC 891756' #TrackingRef '- kbss.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H90 N18 O10' _chemical_formula_weight 1535.76 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' O O 0.0106 0.0060 '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 12.2782(16) _cell_length_b 13.2135(17) _cell_length_c 14.5513(18) _cell_angle_alpha 112.161(4) _cell_angle_beta 90.663(4) _cell_angle_gamma 112.966(4) _cell_volume 1977.9(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24130 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.978 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD APEX 2' _diffrn_measurement_method hemisphere _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25130 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7641 _reflns_number_gt 5021 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7641 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1828 _refine_ls_goodness_of_fit_ref 1.223 _refine_ls_restrained_S_all 1.223 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 C1A C 1.32776(19) 0.70500(19) -0.29572(16) 0.0416(5) Uani 1 1 d . . . H1A H 1.2931 0.6992 -0.3595 0.050 Uiso 1 1 calc R . . C3A C 1.22707(19) 0.66562(19) -0.23870(16) 0.0407(5) Uani 1 1 d . . . H3A H 1.2577 0.6437 -0.1900 0.049 Uiso 1 1 calc R . . C2A C 1.24705(19) 0.8002(2) -0.18172(17) 0.0430(5) Uani 1 1 d . . . H2A H 1.2528 0.8257 -0.1086 0.052 Uiso 1 1 calc R . . C4A C 1.37274(19) 0.8382(2) -0.21350(17) 0.0436(5) Uani 1 1 d . . . H4A H 1.3856 0.8956 -0.2441 0.052 Uiso 1 1 calc R . . N11A N 1.50668(16) 0.67608(17) -0.35655(14) 0.0469(5) Uani 1 1 d . . . H11A H 1.5341 0.7369 -0.3722 0.056 Uiso 1 1 calc R . . N12A N 1.38826(17) 0.54557(17) -0.29935(14) 0.0464(5) Uani 1 1 d . . . C11A C 1.40743(19) 0.6427(2) -0.31563(16) 0.0411(5) Uani 1 1 d . . . C12A C 1.4807(2) 0.5140(2) -0.33287(16) 0.0454(6) Uani 1 1 d . . . C13A C 1.5556(2) 0.5960(2) -0.36858(16) 0.0464(6) Uani 1 1 d . . . C14A C 1.6550(2) 0.5849(3) -0.40722(19) 0.0613(7) Uani 1 1 d . . . H14A H 1.7052 0.6393 -0.4311 0.074 Uiso 1 1 calc R . . C15A C 1.6759(3) 0.4895(3) -0.4085(2) 0.0700(8) Uani 1 1 d . . . H15A H 1.7422 0.4798 -0.4335 0.084 Uiso 1 1 calc R . . C16A C 1.6019(3) 0.4078(3) -0.3739(2) 0.0680(8) Uani 1 1 d . . . H16A H 1.6192 0.3444 -0.3761 0.082 Uiso 1 1 calc R . . C17A C 1.5028(2) 0.4185(2) -0.33596(19) 0.0599(7) Uani 1 1 d . . . H17A H 1.4525 0.3630 -0.3132 0.072 Uiso 1 1 calc R . . N21A N 1.17642(19) 0.8640(2) -0.30324(17) 0.0601(6) Uani 1 1 d . . . N22A N 1.06286(16) 0.83548(17) -0.19023(15) 0.0479(5) Uani 1 1 d . . . H22A H 1.0392 0.8195 -0.1399 0.058 Uiso 1 1 calc R . . C21A C 1.1638(2) 0.8347(2) -0.22554(17) 0.0449(5) Uani 1 1 d . . . C22A C 1.0047(2) 0.8665(2) -0.24910(19) 0.0476(6) Uani 1 1 d . . . C23A C 1.0754(2) 0.8839(2) -0.3194(2) 0.0558(6) Uani 1 1 d . . . C24A C 1.0412(3) 0.9168(3) -0.3911(3) 0.0849(10) Uani 1 1 d . . . H24A H 1.0883 0.9297 -0.4387 0.102 Uiso 1 1 calc R . . C25A C 0.9353(3) 0.9298(3) -0.3892(3) 0.0845(10) Uani 1 1 d . . . H25A H 0.9104 0.9512 -0.4369 0.101 Uiso 1 1 calc R . . C26A C 0.8649(3) 0.9119(3) -0.3185(3) 0.0730(8) Uani 1 1 d . . . H26A H 0.7939 0.9215 -0.3197 0.088 Uiso 1 1 calc R . . C27A C 0.8976(2) 0.8804(2) -0.2466(2) 0.0637(7) Uani 1 1 d . . . H27A H 0.8508 0.8688 -0.1985 0.076 Uiso 1 1 calc R . . N31A N 0.88403(19) 0.3699(2) -0.39242(18) 0.0607(6) Uani 1 1 d . . . C31A C 0.9761(3) 0.3957(3) -0.4390(2) 0.0665(8) Uani 1 1 d . . . H31A H 0.9651 0.3461 -0.5070 0.080 Uiso 1 1 calc R . . C32A C 1.0862(2) 0.4903(2) -0.39405(19) 0.0603(7) Uani 1 1 d . . . H32A H 1.1475 0.5035 -0.4311 0.072 Uiso 1 1 calc R . . C33A C 1.1061(2) 0.5663(2) -0.29327(17) 0.0418(5) Uani 1 1 d . . . C34A C 1.0107(2) 0.5402(2) -0.24479(19) 0.0549(6) Uani 1 1 d . . . H34A H 1.0192 0.5888 -0.1770 0.066 Uiso 1 1 calc R . . C35A C 0.9029(2) 0.4430(2) -0.2953(2) 0.0611(7) Uani 1 1 d . . . H35A H 0.8401 0.4275 -0.2600 0.073 Uiso 1 1 calc R . . N41A N 1.6929(2) 0.9439(2) -0.0095(2) 0.0743(7) Uani 1 1 d . . . C41A C 1.5857(3) 0.8764(2) 0.0008(2) 0.0689(8) Uani 1 1 d . . . H41A H 1.5818 0.8508 0.0526 0.083 Uiso 1 1 calc R . . C42A C 1.4789(2) 0.8412(2) -0.0599(2) 0.0562(7) Uani 1 1 d . . . H42A H 1.4061 0.7939 -0.0483 0.067 Uiso 1 1 calc R . . C43A C 1.4810(2) 0.8765(2) -0.13785(17) 0.0461(6) Uani 1 1 d . . . C44A C 1.5929(2) 0.9480(2) -0.1485(2) 0.0600(7) Uani 1 1 d . . . H44A H 1.6000 0.9755 -0.1994 0.072 Uiso 1 1 calc R . . C45A C 1.6938(2) 0.9784(3) -0.0833(2) 0.0702(8) Uani 1 1 d . . . H45A H 1.7680 1.0268 -0.0920 0.084 Uiso 1 1 calc R . . C1B C 1.5436(2) 1.4516(2) 0.02175(18) 0.0487(6) Uani 1 1 d . . . H1B H 1.5338 1.4420 0.0851 0.058 Uiso 1 1 calc R . . C2B C 1.5806(2) 1.5877(2) 0.04042(17) 0.0476(6) Uani 1 1 d . . . H2B H 1.5850 1.6361 0.1117 0.057 Uiso 1 1 calc R . . N11B N 1.73141(18) 1.42326(19) 0.01152(17) 0.0560(5) Uani 1 1 d . . . H11B H 1.7676 1.4762 0.0717 0.067 Uiso 1 1 calc R . . N12B N 1.58725(19) 1.30980(19) -0.12506(17) 0.0592(6) Uani 1 1 d . . . C11B C 1.6186(2) 1.3930(2) -0.03217(19) 0.0512(6) Uani 1 1 d . . . C12B C 1.6872(2) 1.2836(2) -0.1438(2) 0.0611(7) Uani 1 1 d . . . C13B C 1.7777(2) 1.3542(2) -0.0576(2) 0.0588(7) Uani 1 1 d . . . C14B C 1.8868(3) 1.3459(3) -0.0560(3) 0.0789(9) Uani 1 1 d . . . H14B H 1.9480 1.3925 0.0007 0.095 Uiso 1 1 calc R . . C15B C 1.8994(4) 1.2637(4) -0.1444(4) 0.0989(13) Uani 1 1 d . . . H15B H 1.9710 1.2548 -0.1460 0.119 Uiso 1 1 calc R . . C16B C 1.8110(4) 1.1952(3) -0.2293(3) 0.0919(11) Uani 1 1 d . . . H16B H 1.8248 1.1432 -0.2870 0.110 Uiso 1 1 calc R . . C17B C 1.7039(3) 1.2023(3) -0.2301(3) 0.0771(9) Uani 1 1 d . . . H17B H 1.6431 1.1541 -0.2870 0.092 Uiso 1 1 calc R . . N21B N 1.90053(19) 1.7667(2) -0.05856(18) 0.0644(6) Uani 1 1 d . . . C21B C 1.8853(2) 1.8085(3) 0.0366(2) 0.0640(7) Uani 1 1 d . . . H21B H 1.9467 1.8796 0.0831 0.077 Uiso 1 1 calc R . . C22B C 1.7846(2) 1.7533(2) 0.07063(19) 0.0530(6) Uani 1 1 d . . . H22B H 1.7805 1.7862 0.1387 0.064 Uiso 1 1 calc R . . C23B C 1.6907(2) 1.6506(2) 0.00500(17) 0.0453(6) Uani 1 1 d . . . C24B C 1.7034(2) 1.6086(2) -0.09559(18) 0.0545(6) Uani 1 1 d . . . H24B H 1.6415 1.5401 -0.1442 0.065 Uiso 1 1 calc R . . C25B C 1.8077(2) 1.6685(3) -0.1225(2) 0.0620(7) Uani 1 1 d . . . H25B H 1.8138 1.6382 -0.1902 0.074 Uiso 1 1 calc R . . O1W O 1.46169(17) 1.12754(18) -0.59724(15) 0.0731(6) Uani 1 1 d . . . O1M O 1.22379(19) 0.40893(19) -0.21700(15) 0.0708(6) Uani 1 1 d . . . H1M H 1.277(2) 0.452(2) -0.2451(18) 0.050 Uiso 1 1 d . . . C1M C 1.1517(3) 0.2970(3) -0.2972(3) 0.0916(10) Uani 1 1 d . . . H1M1 H 1.1705 0.3001 -0.3602 0.137 Uiso 1 1 calc R . . H1M2 H 1.0683 0.2800 -0.2965 0.137 Uiso 1 1 calc R . . H1M3 H 1.1671 0.2344 -0.2895 0.137 Uiso 1 1 calc R . . O2W O 1.30383(15) 0.83761(17) -0.46618(14) 0.0661(5) Uani 1 1 d . . . O3W O 1.3111(2) 1.0454(3) -0.4820(2) 0.1156(9) Uani 1 1 d . . . O4W O 1.3674(3) 1.1415(3) -0.2722(2) 0.1258(10) 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 C1A 0.0404(12) 0.0447(12) 0.0436(12) 0.0205(10) 0.0115(10) 0.0199(10) C3A 0.0418(12) 0.0440(12) 0.0457(12) 0.0243(10) 0.0141(10) 0.0221(10) C2A 0.0427(12) 0.0464(12) 0.0462(12) 0.0223(10) 0.0142(10) 0.0220(10) C4A 0.0426(12) 0.0431(12) 0.0530(13) 0.0244(11) 0.0151(10) 0.0214(10) N11A 0.0419(10) 0.0482(11) 0.0528(11) 0.0232(9) 0.0157(9) 0.0189(9) N12A 0.0454(11) 0.0512(11) 0.0512(11) 0.0244(9) 0.0160(9) 0.0256(9) C11A 0.0390(12) 0.0444(12) 0.0411(11) 0.0187(10) 0.0124(9) 0.0179(10) C12A 0.0455(13) 0.0512(13) 0.0429(12) 0.0157(11) 0.0106(10) 0.0275(11) C13A 0.0417(12) 0.0555(14) 0.0414(12) 0.0136(11) 0.0095(10) 0.0265(11) C14A 0.0491(14) 0.0818(19) 0.0549(15) 0.0240(14) 0.0171(12) 0.0336(14) C15A 0.0666(18) 0.096(2) 0.0587(16) 0.0211(16) 0.0182(14) 0.0564(18) C16A 0.079(2) 0.079(2) 0.0604(16) 0.0207(15) 0.0138(15) 0.0558(17) C17A 0.0662(17) 0.0595(16) 0.0600(15) 0.0208(13) 0.0119(13) 0.0363(14) N21A 0.0608(13) 0.0853(16) 0.0698(14) 0.0495(13) 0.0323(11) 0.0486(12) N22A 0.0448(11) 0.0546(12) 0.0570(12) 0.0289(10) 0.0221(9) 0.0275(9) C21A 0.0443(13) 0.0456(13) 0.0515(13) 0.0221(11) 0.0174(11) 0.0237(10) C22A 0.0427(13) 0.0426(13) 0.0618(14) 0.0213(11) 0.0147(11) 0.0226(10) C23A 0.0529(15) 0.0673(16) 0.0706(16) 0.0400(14) 0.0202(13) 0.0372(13) C24A 0.082(2) 0.130(3) 0.099(2) 0.082(2) 0.0380(19) 0.067(2) C25A 0.079(2) 0.101(3) 0.116(3) 0.068(2) 0.019(2) 0.057(2) C26A 0.0550(17) 0.0713(19) 0.110(2) 0.0454(18) 0.0142(17) 0.0362(15) C27A 0.0504(15) 0.0595(16) 0.090(2) 0.0318(15) 0.0211(14) 0.0313(13) N31A 0.0487(12) 0.0589(13) 0.0717(15) 0.0280(12) 0.0079(11) 0.0196(10) C31A 0.0602(17) 0.0690(18) 0.0546(15) 0.0195(14) 0.0062(13) 0.0183(14) C32A 0.0492(15) 0.0701(17) 0.0527(15) 0.0242(13) 0.0143(12) 0.0179(13) C33A 0.0426(12) 0.0437(12) 0.0492(13) 0.0249(11) 0.0122(10) 0.0228(10) C34A 0.0499(14) 0.0538(14) 0.0574(14) 0.0215(12) 0.0184(12) 0.0199(12) C35A 0.0485(15) 0.0565(15) 0.0779(18) 0.0297(14) 0.0235(13) 0.0198(12) N41A 0.0570(15) 0.0629(15) 0.0840(18) 0.0098(14) -0.0059(13) 0.0275(12) C41A 0.0704(19) 0.0553(16) 0.0769(19) 0.0243(14) -0.0060(15) 0.0263(15) C42A 0.0518(15) 0.0462(14) 0.0672(16) 0.0256(13) 0.0020(12) 0.0158(11) C43A 0.0445(13) 0.0399(12) 0.0522(13) 0.0138(11) 0.0108(11) 0.0214(10) C44A 0.0467(15) 0.0572(15) 0.0631(16) 0.0174(13) 0.0141(13) 0.0166(12) C45A 0.0448(15) 0.0675(18) 0.0726(19) 0.0117(16) 0.0101(14) 0.0154(13) C1B 0.0478(14) 0.0559(14) 0.0512(13) 0.0281(11) 0.0195(11) 0.0247(11) C2B 0.0466(13) 0.0521(13) 0.0461(12) 0.0197(11) 0.0159(10) 0.0233(11) N11B 0.0518(13) 0.0615(13) 0.0650(13) 0.0336(11) 0.0185(10) 0.0269(10) N12B 0.0513(12) 0.0552(13) 0.0736(15) 0.0274(12) 0.0212(11) 0.0242(10) C11B 0.0488(14) 0.0504(14) 0.0638(16) 0.0311(13) 0.0205(12) 0.0229(11) C12B 0.0618(17) 0.0556(15) 0.0856(19) 0.0392(15) 0.0370(15) 0.0340(14) C13B 0.0596(16) 0.0619(16) 0.0810(18) 0.0458(15) 0.0334(15) 0.0350(14) C14B 0.0653(19) 0.106(2) 0.106(2) 0.070(2) 0.0330(18) 0.0510(18) C15B 0.107(3) 0.134(3) 0.143(4) 0.096(3) 0.078(3) 0.099(3) C16B 0.105(3) 0.084(2) 0.121(3) 0.049(2) 0.058(3) 0.067(2) C17B 0.087(2) 0.0603(17) 0.092(2) 0.0315(16) 0.0389(18) 0.0390(16) N21B 0.0500(13) 0.0742(15) 0.0733(15) 0.0390(13) 0.0232(12) 0.0223(12) C21B 0.0502(15) 0.0607(16) 0.0721(18) 0.0286(14) 0.0095(13) 0.0138(13) C22B 0.0557(15) 0.0540(14) 0.0498(13) 0.0216(12) 0.0120(12) 0.0237(12) C23B 0.0446(13) 0.0470(13) 0.0525(13) 0.0235(11) 0.0165(11) 0.0245(11) C24B 0.0487(14) 0.0568(15) 0.0522(14) 0.0200(12) 0.0138(11) 0.0192(12) C25B 0.0643(17) 0.0734(18) 0.0546(15) 0.0296(14) 0.0254(13) 0.0321(15) O1W 0.0728(13) 0.0736(13) 0.0778(13) 0.0414(11) 0.0156(10) 0.0264(10) O1M 0.0742(13) 0.0729(13) 0.0692(12) 0.0392(11) 0.0253(11) 0.0255(11) C1M 0.088(2) 0.082(2) 0.094(2) 0.040(2) 0.007(2) 0.0220(19) O2W 0.0533(11) 0.0691(12) 0.0714(12) 0.0302(10) 0.0188(9) 0.0205(9) O3W 0.109(2) 0.122(2) 0.143(2) 0.0811(19) 0.0525(18) 0.0497(17) O4W 0.129(2) 0.112(2) 0.119(2) 0.0374(17) 0.0040(18) 0.0442(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 C1A C11A 1.475(3) . ? C1A C3A 1.528(3) . ? C1A C4A 1.572(3) . ? C3A C33A 1.491(3) . ? C3A C2A 1.566(3) . ? C2A C21A 1.491(3) . ? C2A C4A 1.560(3) . ? C4A C43A 1.501(3) . ? N11A C11A 1.353(3) . ? N11A C13A 1.368(3) . ? N12A C11A 1.324(3) . ? N12A C12A 1.388(3) . ? C12A C17A 1.376(4) . ? C12A C13A 1.396(3) . ? C13A C14A 1.386(3) . ? C14A C15A 1.375(4) . ? C15A C16A 1.379(4) . ? C16A C17A 1.377(4) . ? N21A C21A 1.319(3) . ? N21A C23A 1.399(3) . ? N22A C21A 1.350(3) . ? N22A C22A 1.375(3) . ? C22A C23A 1.377(3) . ? C22A C27A 1.395(3) . ? C23A C24A 1.389(4) . ? C24A C25A 1.376(4) . ? C25A C26A 1.380(4) . ? C26A C27A 1.372(4) . ? N31A C31A 1.321(3) . ? N31A C35A 1.332(3) . ? C31A C32A 1.365(4) . ? C32A C33A 1.381(3) . ? C33A C34A 1.370(3) . ? C34A C35A 1.371(3) . ? N41A C45A 1.314(4) . ? N41A C41A 1.319(4) . ? C41A C42A 1.379(4) . ? C42A C43A 1.378(4) . ? C43A C44A 1.381(3) . ? C44A C45A 1.377(4) . ? C1B C11B 1.476(3) . ? C1B C2B 1.552(3) 2_885 ? C1B C2B 1.583(3) . ? C2B C23B 1.499(3) . ? C2B C1B 1.552(3) 2_885 ? N11B C11B 1.356(3) . ? N11B C13B 1.376(3) . ? N12B C11B 1.312(3) . ? N12B C12B 1.403(3) . ? C12B C17B 1.391(4) . ? C12B C13B 1.398(4) . ? C13B C14B 1.387(4) . ? C14B C15B 1.393(5) . ? C15B C16B 1.371(5) . ? C16B C17B 1.355(5) . ? N21B C25B 1.327(3) . ? N21B C21B 1.329(3) . ? C21B C22B 1.374(4) . ? C22B C23B 1.363(3) . ? C23B C24B 1.391(3) . ? C24B C25B 1.368(4) . ? O1M C1M 1.409(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 C11A C1A C3A 117.26(19) . . ? C11A C1A C4A 121.11(18) . . ? C3A C1A C4A 88.78(16) . . ? C33A C3A C1A 121.28(18) . . ? C33A C3A C2A 122.11(19) . . ? C1A C3A C2A 89.58(16) . . ? C21A C2A C4A 113.33(19) . . ? C21A C2A C3A 115.14(19) . . ? C4A C2A C3A 87.85(16) . . ? C43A C4A C2A 117.95(19) . . ? C43A C4A C1A 113.35(18) . . ? C2A C4A C1A 88.22(16) . . ? C11A N11A C13A 107.9(2) . . ? C11A N12A C12A 105.12(18) . . ? N12A C11A N11A 112.19(19) . . ? N12A C11A C1A 124.36(19) . . ? N11A C11A C1A 123.4(2) . . ? C17A C12A C13A 120.7(2) . . ? C17A C12A N12A 129.8(2) . . ? C13A C12A N12A 109.4(2) . . ? N11A C13A C14A 133.2(2) . . ? N11A C13A C12A 105.40(19) . . ? C14A C13A C12A 121.4(2) . . ? C15A C14A C13A 116.7(3) . . ? C14A C15A C16A 122.2(3) . . ? C17A C16A C15A 121.0(3) . . ? C16A C17A C12A 117.9(3) . . ? C21A N21A C23A 105.0(2) . . ? C21A N22A C22A 107.8(2) . . ? N21A C21A N22A 112.1(2) . . ? N21A C21A C2A 125.5(2) . . ? N22A C21A C2A 122.4(2) . . ? N22A C22A C23A 105.6(2) . . ? N22A C22A C27A 132.1(2) . . ? C23A C22A C27A 122.4(2) . . ? C24A C23A C22A 120.0(2) . . ? C24A C23A N21A 130.4(2) . . ? C22A C23A N21A 109.6(2) . . ? C23A C24A C25A 117.8(3) . . ? C26A C25A C24A 121.7(3) . . ? C27A C26A C25A 121.4(3) . . ? C26A C27A C22A 116.7(3) . . ? C31A N31A C35A 116.2(2) . . ? N31A C31A C32A 124.3(3) . . ? C31A C32A C33A 119.6(2) . . ? C34A C33A C32A 116.2(2) . . ? C34A C33A C3A 121.9(2) . . ? C32A C33A C3A 121.8(2) . . ? C35A C34A C33A 120.7(2) . . ? N31A C35A C34A 123.0(2) . . ? C45A N41A C41A 115.6(3) . . ? N41A C41A C42A 124.5(3) . . ? C41A C42A C43A 119.5(3) . . ? C44A C43A C42A 116.3(2) . . ? C44A C43A C4A 118.6(2) . . ? C42A C43A C4A 125.0(2) . . ? C43A C44A C45A 119.4(3) . . ? N41A C45A C44A 124.7(3) . . ? C11B C1B C2B 115.6(2) . 2_885 ? C11B C1B C2B 117.65(19) . . ? C2B C1B C2B 90.82(18) 2_885 . ? C23B C2B C1B 117.4(2) . 2_885 ? C23B C2B C1B 118.61(19) . . ? C1B C2B C1B 89.18(18) 2_885 . ? C11B N11B C13B 107.8(2) . . ? C11B N12B C12B 105.1(2) . . ? N12B C11B N11B 112.7(2) . . ? N12B C11B C1B 125.6(2) . . ? N11B C11B C1B 121.7(2) . . ? C17B C12B C13B 120.8(3) . . ? C17B C12B N12B 129.9(3) . . ? C13B C12B N12B 109.3(2) . . ? N11B C13B C12B 105.1(2) . . ? N11B C13B C14B 133.8(3) . . ? C12B C13B C14B 121.0(3) . . ? C15B C14B C13B 116.0(3) . . ? C16B C15B C14B 123.0(3) . . ? C17B C16B C15B 120.9(3) . . ? C16B C17B C12B 118.3(3) . . ? C25B N21B C21B 115.3(2) . . ? N21B C21B C22B 124.2(3) . . ? C23B C22B C21B 120.2(2) . . ? C22B C23B C24B 116.2(2) . . ? C22B C23B C2B 121.3(2) . . ? C24B C23B C2B 122.5(2) . . ? C25B C24B C23B 119.6(2) . . ? N21B C25B C24B 124.5(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.627 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.049